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Analytical tasks – efficiently solved by HPTLC

Boswellia resin

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CAMAG BIBLIOGRAPHY SERVICE

No. 104, March 2010CAMAG Bibliography Service Planar Chromatography Edited by Gerda Morlock cbs@camag.com published by CAMAG Switzerland

CAMAG (Switzerland) Sonnenmattstr. 11 • CH-4132 Muttenz 1 Tel. +41 61 4673434 • Fax +41 61 4610702 info@camag.com • www.camag.com

CAMAG Scientific Inc. (USA) 515 Cornelius Harnett Drive Wilmington, NC 28401 Phone 800 334 3909 • Fax 910 343 1834 tlc@camagusa.com • www.camagusa.com

IN THIS ISSUE

Procedures, applicationsA comparison between HPLC and HPTLC for the separation and quantification of boswellic acids in Boswellia serrata extracts ......... 2–4

Validated HPTLC method for skin lipids ............................... 5–6

Separation of common plant triterpenoids by HPTLC ........ 7–9

Validated determination of secoisolariciresinol diglucoside in flaxseed by HPTLC ................. 10–12

Determination of aloe vera gels in cosmetics .............................. 13–15

Products featured in this issue Horizontal Developing Chamber ....... 11

Automatic TLC Sampler (ATS 4) ........ 15

New TLC Scanner 4 ....................... 16

Column: Know CAMAGOnline Coupling of HPTLC-MS on the road to success ...................... 8

Printed on FSC/PEFC-certified paper

Planar Chromatography in Practice

A comparison between HPLC and HPTLC for the separation and quantification of boswellic acids in Boswellia serrata extracts

The Department of Standardization and New Technologies of the Saint Petersburg Institute of Pharmacy was introduced in CBS 102. In their daily routine, HPTLC is especially helpful for the optimization of the extraction, determination of antiradical activity, or the study of the kinetics of active metabolites in plasma. They currently use more than 20 validated, quan-titative HPTLC methods, such as quantification of chlorogenic, caffeic and ferulic acids in coffee bean extracts, curcuminoids in plasma and dosage forms, bile acids and cholesterol in the bile of rats, etc.

IntroductionBoswellia serrata Roxb. (Indian frankincense) is an Indian medical plant and its gum resin is used as an antipyretic, analgesic, diuretic, or antidysenteric traditional medicine, among other usages. The anti-inflammatory and an-tiarthritic activity of its extracts has been tested in animal experiments and in clinical trials [1, 2]. The main active compounds of Boswellia serrata ex-tracts are triterpenic acids [2] like -boswellic acid (BA), acetyl--boswellic acid (ABA), 11-keto--boswellic acid (KBA) and acetyl-11-keto--boswellic acid (AKBA). For the analysis of boswellic acids, a nonaqueous titration method [3], HPLC [4], GC–MS [5], LC–MS [6], and HPTLC methods [7] have been reported.

The aim of this work was to compare the capabilities of two chro-matographic methods, HPTLC and HPLC, for identification and quantification of the four major boswellic acids in Boswellia ser-rata extracts.

Left to right: Prof. Alexander Shikov*, Dr. Olga Pozharitskaya, Dr. Svetlana Ivanova, Prof. Valery Makarov, Dr. Vera Kosman

CBS 104 3

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Chromatogram layer and HPLC column• HPTLC plates silica gel 60 F254, 10 x 10 cm (Merck).

• HPLC column Luna C18 (150 x 4.6 mm, 5 µm, Phenomenex, USA) and a SecurityGuard 20-mm precolumn with the same sorbent

Standard solutionsMethanolic solutions (0.5 mg/mL) of BA, ABA, KBA, and AKBA were used.

Sample preparationCommercially available standardized Boswellia ser-rata extracts were a kind gift from New Ambadi Estates Pvt. Ltd. (Chennai, India). Sample solutions were prepared by dissolving of the Boswellia serrata extracts in methanol (10 mg/mL).

Sample application and HPLC injection• Bandwise with Linomat 5, band length 6 mm, dis-

tance from lower edge 10 mm, distance on both sides min. 10 mm, application volumes 1–20 µL

• Injection volume of 20 µL for HPLC analysis

Chromatography• In the Twin-Trough Chamber pre-saturated (for

15 min, using wetted filter paper) with n-hexane – ethyl acetate – glacial acetic acid 16:5:1 up to a migration distance of 7 cm (ca. 10 min)

• HPLC (Waters Inc., USA) consisting of two 510 series pumps, an automated gradient controller and a 484 model tunable absorbance detector. Separation was carried out at room temperature with a flow rate of 1 mL/min using a 20-min linear gradient from 75 % to 100 % acetonitrile (other phase: 0.03 % aqueous trifluoroacetic acid solu-tion), followed by a 15-min isocratic step.

Densitometry• Absorption measurement at 254 nm for KBA and

AKBA, and after derivatization at 560 nm for BA and ABA using TLC Scanner 3 and winCats soft-ware.

• HPLC-UV detection at 254 nm for KBA and AKBA and at 210 nm for BA and ABA.

Post-chromatographic derivatizationFor visualization of BA and ABA, the plate was manu-ally dipped in anisaldehyde sulfuric acid reagent (1 mL anisaldehyde and 2 mL conc. sulfuric acid in 100 mL glacial acetic acid) followed by heating at 110 °C for 5 min on the TLC plate heater.

Note (editor): Using automated immersion by the TLC Chroma-togram Immersion Device (immersion time 1 s, vertical speed 3.5 cm/s) will improve the precision.

HPTLC densitogram at 254 nm of BA (track 1), ABA (track 2), AKBA (track 3), KBA (track 4), and two B. serrata extracts (track 5 and 6)

Visualization by anisaldehyde sulfuric acid reagent: tracks 1 and 2 B. serrata extract at 5 and 10 µg/band, track 3 BA, and track 4 ABA

Results and discussionFor both methods, quantification of boswellic acids by external standard calibration was performed, and both methods were validated according to the ICH guidelines on the validation of analytical methods. Using a 20-µL volume for injection in HPLC, the limits of detection (LOD) for KBA and AKBA were

4 CBS 104

The two methods treated as paired data were compared by the matched pair Student‘s t-test. The calculated t-values were between 2.16 and 2.45 for the different boswellic acids and below the t-table value of 2.57. Hence, it was concluded that both methods gave identical results for the analysis of boswellic acids in the extracts. There was no statisti-cally significant difference (P = 99 %) between the mean values for all extracts. Considering the fast analysis time, low solvent consumption and high sample throughput capacity, HPTLC is the method of choice for routine analysis.

Results of HPLC and HPTLC quantification of boswellic acids in Boswellia extracts

Compound Sample 1 (%, w/w)a Sample 2 (%, w/w)a

HPLC HPTLC HPLC HPTLC

BA 18.9 ± 1.2 19.0 ± 1.7 22.4 ± 0.7 23.4 ± 1.9

ABA 11.9 ± 1.2 12.4 ± 1.4 11.6 ± 0.3 12.3 ± 1.2

KBA 3.8 ± 0.6 3.4 ± 0.1 8.0 ± 0.1 7.7 ± 0.1

AKBA 3.9 ± 0.7 3.6 ± 0.1 5.1 ± 0.2 5.2 ± 0.1

Total 38.5 37.9 47.1 48.6

a ± standard deviation (n = 3) expressed on dry weight

Boswellic acids:

BA with R = a-OH KBA with R = a-OH

ABA with R = a-CH3COO AKBA with R = a-CH3COO

Further information is available on request from the authors.

[1] T. Syrovets et al. J. Immunol. 174 (2005) 498

[2] B.A. Shah et al. Nat. Prod. Rep. 26 (2009) 72

[3] R.K. Gupta et al. Indian Drugs 21 (1984) 523

[4] B. Buchele and T. Simmet J. Chromatography B 795 (2003) 355

[5] A. Kaunzinger et al. J. Pharm. Biomed. Anal. 28 (2002) 729

[6] K. Reising et al. Anal. Chem. 77 (2005) 6640

[7] O.N. Pozharitskaya et al. J. Sep. Sci. 29 (2006) 2245

* Prof. Dr. Alexander Shikov, Saint Petersburg Institute of Phar- macy, 47/5, Piskarevsky prospect, 195067, St. Petersburg, Russia, spb.pharmacy@gmail.com

6–8 ng and for BA and ABA 60–80 ng. In HPTLC just a 2-µL volume was applied. LOD obtained were 150 ng for KBA and AKBA and 100 ng for BA and ABA. If required, LOD can be improved using a higher volume for application. Regarding precision, the relative standard deviations (%RSD) of boswellic acids varied from 6 to 18 % using HPLC. For HPTLC, %RSD of AKBA and KBA were ≤ 2 %, and after derivatization, for BA and ABA about 10 %, which could be improved by automated immersion.

Two differently marketed, dry Boswellia serrata extracts were analyzed in triplicate using both methods.

CBS 104 5

CAMAG Laboratory: Method Development in Practice

Validated HPTLC method for skin lipids

Karin Rothenbühler

In cooperation with the University of Basel and under supervision of Prof. Matthias Hamburger, Ms. Karin Rothenbühler has worked on her master thesis [1] in Pharmaceutical Biology at the CAMAG laboratory.

IntroductionEven though numerous literature references indi-cate that TLC/HPTLC is the method of choice for skin lipid analysis, no validated quantitative HPTLC method was found. Following the recent publica-tion on the HPTLC analysis of phospholipids [2], Ms. Rothenbühler developed and validated a HPTLC method for the most important markers of non-polar lipid classes of the human stratum corneum: squalene, triolein, palmitic acid, 1,2-dipalmitoyl-sn-glycerol, stearyl palmitate, cholesteryl palmitate, and cholesterol.

In combination with appropriate sampling procedures the method was rapid, robust and reliable for use by the R&D laboratories of cosmetic industry. The advantages of HPTLC, in comparison to RP-HPLC, are its simple derivati-zation as a prerequisite for lipid detection and the separation based on functional groups.

Sample preparationSkin samples were obtained from the inner forearm of volunteers either by direct extraction with etha-nol, abrasion of a defined area with a razor blade or with Epiglu, a tissue adhesive for medicinal use.

Standard solutions2 mg each of squalene, triolein, palmitic acid, 1,2-dipalmitoyl-sn-glycerol, stearyl palmitate, cholesteryl palmitate, and cholesterol were dissolved in 10 mL of

chloroform – methanol 1:1. For quantification 1 mL of this solution was diluted with 4 mL of chloroform – methanol 1:1.

Chromatogram layerHPTLC plates LiChrospher silica gel 60 F254 (Merck), 20 × 10 cm, pre-washed by developing with metha-nol followed by drying in an oven at 120 °C for 20 min.

Sample applicationBandwise with ATS4, band length 8 mm, track dis-tance min. 10 mm, distance from lower edge 8 mm, distance from left edge min. 15 mm, application volumes 2–30 µL of samples and 2.5–10 µL of standard solutions.

ChromatographyIn the ADC2 with chamber saturation for 20 min first with toluene to a migration distance of 80 mm followed by drying for 5 min, then with n-hexane, t-butyl methyl ether, acetic acid 80:20:1 to 45 mm. Separation was affected by the plate activity, there-fore plates were conditioned prior to both develop-ments at 33 % relative humidity for 10 min using a saturated solution of magnesium chloride.

Post-chromatographic derivatizationCopper(II) sulfate reagent was prepared by dissolving 20 g Copper(II) sulfate pentahydrate in 200 mL of cooled methanol and then adding 8 mL of sulphuric acid 98 % and 8 mL of orthophosphoric acid 85 %. With the Immersion Device III the plate was dipped for 6 s into the reagent, then dried for 30 s with cold air and finally heated on a plate heater for 30 min at 140 °C.

DensitometryTLC Scanner 3 with winCATS software, absorption measurement at 350 nm.

Results and discussionSince there was no standardized methodology for sampling of human skin samples, various tech-niques were evaluated. Skin samples from the in-ner forearm of volunteers were obtained by use of various commercial tapes, medicinal tissue adhesive,

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The major challenge involved with the use of tapes and glues was to selectively extract the skin lipids from the carrier ma-terial, whereas the direct application of organic solvents was limited to ethanol to avoid skin irritations. Three sampling methods (direct extraction with ethanol, abrasion, Epiglu) were suitable for quantitative investigations, as neither skin nor glue matrix interfered with the lipid zones. However, standardization of the sampling procedure was still difficult because the depth of skin removed (number of stratum cor-neum layers) was unclear and the area of treated skin was difficult to define; further investigations are under way.

Sampling A) by direct abrasion and B) with Epiglu; track 1: lipid standard mix, 2–7: skin lipid samples, 8–9: Epiglu blanks

Standards (track 1: cholesterol, 2: triolein, 3: stearyl palmitate*, 4: ceramid VI, 5: squalene, 6: cholesteryl palmitate*, 7: palmitic acid, 8: 1,2 dipalmitoyl-sn-glycerol) and various extracts of skin lipids (track 9: using ethanol, 10: cyclohexane – ethanol 1:9, 11: cyclohexane – ethanol 1:4, 12: n-hexane – methanol 2:3)*encircled, other zones are impurities

abrasion with a razor blade, cold wax, aluminium foil, cling film or by direct application of organic solvents.

The method was validated regarding stability, robustness, pre-cision of RF values and standard determinations as well as linear range. All lipid standards were stable for at least 3 h in chloroform – methanol 1:1 and on the plate prior to development. Stand-ards as well as extracted skin samples were stable during chromatography. The derivatized chromatogram was stable for at least 2 h. The influence of relative humidity on the

Further information is available on request from the authors.

[1] K. Rothenbühler, Master thesis, Institute for Pharmaceutical Biology, University of Basel, 2009

[2] D. Handloser, V. Widmer, E. Reich, J. Liq. Chro-matogr. Rel. Technol. 31 (2008) 1857

separation was evaluated at 5 %, 33 %, 47 %, and 75 % using the ADC 2. For reproducible selectivity, the relative hu-midity must be maintained between 33 % and 47 %. The precision of the RF values of seven compounds was deter-mined between plates (3 plates devel-oped on the same day, followed by one plate each on two different days). Differ-ences of RF values were

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continuation on page 9

Planar Chromatography in Practice

Separation of common plant triterpenoids by HPTLC

Left to right: Dr. Irena Vovk*, Dr. Breda Simonovska and Mitja Martelanc

The Laboratory for Food Chemistry at the National Institute of Chemistry in Ljubljana (www.ki.si) is the leading research group in the field of planar chromatography in Slovenia, providing consulting for industry and other institutions. Research and development activities are primarily focused on the field of nutraceuticals and the development of analytical methods based on chromatographic techniques.

IntroductionTriterpenoids represent a large class of secondary metabolites commonly present in plants, especially in leaf and fruit epicuticular waxes. Some of them exhibit beneficial activities, such as anti-inflamma-tory ones. Therefore, they are of emerging impor-tance as constituents of food supplements and functional foods.

In general HPLC is used for determination of trit-erpenoids, but due to their lack of chromophores and numerous possible isomeric structures, the choice of detector and mobile phases has limita-tions. On the other hand, HPTLC is indispensible in the investigation of triterpenoids, because it provides unique separations with a wealth of potential mobile phases and with possibilities for in situ derivatization, which results in char-acteristic specific coloration and fluorescence of the separated bands [1, 2]. In the investigation of triterpenoids in plant extracts, the proposed HPTLC methods enable easy, fast and inexpen-sive screening. Depending on the sample char-acteristics, quantification is possible.

Standard solutionsStandard solutions and mixtures were prepared in n-propanol (0.1 mg/mL).

Sample preparationFresh tomato fruit and fresh leaves of cabbage, rosemary and sage were immersed into dichlo-romethane. Pulverized oak bark was extracted with the same solvent. After filtration and evaporation of the solvent, final test solutions were prepared in n-propanol with concentrations of 5 mg/mL (cab-bage and rosemary leaves), 30 mg/mL (sage leaves), 10 mg/mL (oak bark) and 2 mg/mL (tomato fruit) [2].

Chromatogram layerHPTLC plates silica gel 60 (Merck), 20 x 10 cm, pre-washed by developing in chloroform – methanol 1:1 and HPTLC plates RP18 (Merck), 20 x 10 cm, prewashed by developing in acetone, followed by drying on the TLC plate heater at 110 °C for 10 minutes.

Sample applicationBandwise with Linomat, band length 6 mm, dis-tance from lower plate edge 5 mm, from left edge 12 mm, track distance 10 mm, application volumes as follows: 6 µL (cabbage leaves), 7 µL (rosemary leaves), 5 µL (sage leaves), 4 µL (oak bark), and 6 µL (tomato), for standard solutions 2-8 µL.

ChromatographyIn the Horizontal Developing Chamber with n-hex-ane – ethyl acetate 5:1 on silica gel plate (develop-ing time 15 min), whereby the conditioning tray was covered with the developing solvent, and with ethyl acetate – acetonitrile 3:2 or acetone – acetonitrile 5:1 on RP18 plate (developing time 17 min), run-ning distance 8 cm

Post-chromatographic derivatizationDried plates were dipped for 2 s in anisaldehyde sul-furic acid reagent (16 mL sulfuric acid and 1 mL p-methoxybenzaldehyde were added to 20 mL acetic acid and 170 mL methanol during cooling with ice water) using the Chromatogram Immersion Device (vertical speed 3.5 cm/s), dried in a stream of warm air and heated at 110 °C with a TLC Plate Heater for

8 CBS 104

Know CAMAG

Online Coupling of HPTLC-MS on the road to success

Success obliges!

CAMAG will offer the same type of seminars in 2010

• 16.04.2010 University of Oldenburg, Prof. Dr. Christoffers, 26111 Oldenburg, Germany

• 03.06.2010 University of Leiden, Prof. Dr. Overkleeft, 2333 CC Leiden, The Netherlands

• 04.06.2010 University of Gent, Prof. Dr. De Spiegeleer, 9000 Gent, Belgium

• 29.06.2010 Technical University of Munich, Prof. Dr. Schieberle, 85345 Munich, Germany

If you are interested please register by E-mail (info@camag-Berlin.de). You will receive detailed information. Attendance is free of charge.

The one-day seminars announced in CBS 102 met with great interest. Between 30 and 35 analysts attended each of the seminars held in 2009 at Langenau, Offenburg, Münster, Berlin, Basle and Vienna. The participants came from companies and institutes where TLC/HPTLC analysis is a part of the daily routine in foods, pharmaceuticals, water, organic synthesis and natural products’ research. The seminar’s aim was to keep the participants informed on the innovative technique of online coupling and its potential.

Competent speakers reported of their own experi-ence: Dr. H. Luftmann (University of Münster), who developed the interface, reported of the history and background and his experience with its application in organic synthesis. Dr. W. Schulz (Zweckverband Landeswasserversorgung in Langenau) presented the use of HPTLC-MS coupling for identification of organic trace substances in raw and drinking water, Prof. Dr. H.-R. Schmutz (University Northwest Switzerland in Muttenz) lectured on HPTLC-MS of drug compounds and plant ingredients and PD Dr. Gerda Morlock (University of Hohenheim in Stutt-gart) covered applications in the field of food and pharmaceutical analysis. A wide range of analytes of different structural groups was shown such as atrazine and its metabolites, metoprolol and its

degradation products, caffeine, paracetamol, ace-tylsalicyl acid, ginsenoides, isopropylthioxanthone, food dyes, ergotamine, pyridinol and harmane.

In the afternoon there were practical demonstra-tions of the interface with the MS systems available in the respective laboratories. Some participants brought sample chromatograms which were suc-cessfully processed. All participants were convinced of the great potential of the new coupling tech-nique with respect to time saving, cost effectiveness and convenience.

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Dear friends

The efficient solution of ana-lytical tasks by HPTLC is the focus of this issue. An abso-lute prerequisite is a sound knowledge of the state-of- the-art technique – a con-clusion drawn also by Pro-fessor Coran (p. 5).

HPTLC is now clearly es-tablished in the laboratory, 35 years after the introduc-tion of the high-performance layers. But in the field, industry as well as regulatory laboratories, we meet many customers still using classical TLC layers and old fashioned procedures. To a large extent this is due to the fact that standard ope-rating procedures are based on classical TLC lay-ers, and that substituting an established proce-dure with HPTLC requires a lot of bureaucracy. Nonetheless, even this appears much better than struggling along for years with inadequate proce-dures and more importantly, suboptimal results.

Outriders for teaching state-of–the-art know-ledge should be university institutes. But unfor-tunately, nowhere is it more apparent than at universities that TLC is just rudimentarily presen- ted to students, if at all! CAMAG strives to up- grade the knowledge of contemporary HPTLC at universities by offering seminars. If you, as a teaching person are interested in a CAMAG seminar at your institute, contact us via info@ camag.com.

An opportunity to see first hand the progress in HPTLC is the attendance of the International Sym-posium on High-Performance Thin-Layer Chroma- tography in Basle, July 6th – 8th, 2011 (last yellow page). Make a note!

Sincerely,

Gerda Morlock cbs@camag.com

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CAMAG LITERATURDIENSTCAMAG BIBLIOGRAPHY SERVICEPLANAR CHROMATOGRAPHY

Liebe Freunde

Das effiziente Lösen analytischer Fragestellungen mit der HPTLC ist Schwerpunkt dieser Ausgabe. Voraussetzung ist, dass das gesamte Instrumen-tarium optimal eingesetzt wird – eine Folgerung, die auch im Beitrag Coran (S. 5) gezogen wird.

Die HPTLC ist heute – 35 Jahre nach Einführung dieser Schichten – längst in der Praxis angekom-men. Unsere zahlreichen Kundenkontakte zeigen allerdings auch, dass ein großer Teil der Prüfvor-schriften in Industrie und Kontrollinstituten noch auf den klassischen DC-Schichten basiert. Dies liegt einerseits am mangelnden Kenntnisstand eines Teils der Anwender, andererseits am büro-kratischen Aufwand, der erforderlich ist, eine DC-Methode auf HPTLC umzustellen. Aber wäre es nicht besser, die noch vorhandenen DC-Metho-den Schritt für Schritt durch die HPTLC mit ihrem großen Potential zu ersetzen, als sich jahrelang im Routinebetrieb mit einer unzulänglichen Prüfvor-schrift abzufinden? Bürokratie darf kein Hemm-schuh für den analytischen Fortschritt sein!

Vorreiter sollten eigentlich die Universitäten sein. Doch gerade dort wird, wenn überhaupt, den Studierenden die Dünnschicht-Chromatographie oft nur in ihrem rudimentären Stand nahe ge-bracht. CAMAG ist bemüht, durch Seminare den Wissensstand zu aktualisieren. Wenn Sie als Lehr- person daran interessiert sind, melden Sie sich bitte unter info@camag-berlin.de

Eine Gelegenheit, Fortschritte in der HPTLC zu er-fahren, ergibt sich beim International Symposium on High-Performance Thin-Layer Chromatography in Basel vom 6. – 8. Juli 2011 (letzte gelbe Seite). Bitte reservieren Sie sich diesen Termin.

Mit freundlichen Grüssen

Gerda Morlock cbs@camag.com

MARCH

2010

THE CBS CLASSIFICATION SYSTEM1. Reviews and books

a) Books on TLC b) Books containing one or several chapters on TLC c) Books containing frequent TLC information spread over several chapters of other information

2. Fundamentals, theory and general a) General b) Thermodynamics and theoretical relationship c) Relationship between structure and chrom. behaviour d) Measurement of physico-chemical and related values e) Optimization of solvent systems f) Validation of methods

3. General techniques (unless they are restricted to the application within one or two classification sections) a) New apparatus/techniques for sample preparation b) Separation material c) New apparatus for sample application/dosage d) New apparatus/techniques for chromatogram development e) New apparatus/techniques for pre- or post- chromatographic derivatization f) New apparatus/techniques for quantitative evaluation g) New apparatus/techniques for other TLC steps (distinguished from section 4)

4. Special techniques a) Automation of sample preparation/application b) Automation of complex chromatogram developing techniques c) Automation, computer application in quantitative chromatogram evaluation d) Combination of TLC with other chromatographic techniques e) Combination of TLC with other (non-chromatogra- phic) techniques...MS, IR...etc.

5. Hydrocarbons and halogen derivatives a) Aliphatic hydrocarbons b) Cyclic hydrocarbons c) Halogen derivatives d) Complex hydrocarbon mixtures

6. Alcohols

7. Phenols

8. Substances containing heterocyclic oxygen a) Flavonoids b) Other compounds with heterocyclic oxygen

9. Oxo compounds, ethers and epoxides

10. Carbohydrates a) Mono- and oligosaccharides, structural studies b) Polysaccharides, mucopolysaccharides, lipopolysaccharides

11. Organic acids and lipids a) Organic acids and simple esters b) Prostaglandins c) Lipids and their constituents d) Lipoproteins and their constituents e) Glycosphingolipids (gangliosides, sulfatides, neutral glycosphingolipids)

12. Organic peroxides

13. Steroids a) Pregnane and androstane derivatives b) Estrogens c) Sterols d) Bile acids and alcohols e) Ecdysones and other insect steroid hormones

14. Steroid glycosides, saponins and other terpenoid glycosides

15. Terpenes and other volatile plant ingredients a) Terpenes b) Essential oils

16. Nitro and nitroso compounds

17. Amines, amides and related nitrogen compounds a) Amines and polyamines b) Catecholamines and their metabolites c) Amino derivatives and amides (excluding peptides)

18. Amino acids and peptides, chemical structure of proteins a) Amino acids and their derivatives b) Peptides and peptidic proteinous hormones

19. Proteins

20. Enzymes

21. Purines, pyrimidines, nucleic acids and their constituents a) Purines, pyrimidines, nucleosides, nucleotides b) Nucleic acids, RNA, DNA

22. Alkaloids

23. Other substances containing heterocyclic nitrogen a) Porphyrins and other pyrroles b) Bile pigments c) Indole derivatives d) Pyridine derivatives e) other N-heterocyclic compounds

24. Organic sulfur compounds

25. Organic phosphorus compounds (other than phospholipids)

26. Organometallic and related compounds a) Organometallic compounds b) Boranes, silanes and related non-metallic compounds c) Coordination compounds

27. Vitamins and various growth regulators (non-peptidic)

28. Antibiotics, Mycotoxins a) Antibiotics b) Aflatoxins and other mycotoxins

29. Pesticides and other agrochemicals a) Chlorinated insecticides b) Phosphorus insecticides c) Carbamates d) Herbicides e) Fungicides f) Other types of pesticides and various agrochemicals

30. Synthetic and natural dyes a) Synthetic dyes b) Chloroplasts and other natural pigments

31. Plastics and their intermediates

32. Pharmaceutical and biomedical applications a) Synthetic drugs b) Pharmacokinetic studies c) Drug monitoring d) Toxicological applications e) Plant extracts, herbal and traditional medicines f) Clinico-chemical applications and profiling body fluids

33. Inorganic substances a) Cations b) Anions

34. Radioactive and other isotopic compounds

35. Other technical products and complex mixtures a) Surfactants b) Antioxidants and preservatives c) Various specific technical products d) Complex mixtures and non-identified compounds

36. Thin-layer electrophoresis

37. Environmental analysis a) General papers b) Air pollution c) Water pollution d) Soil pollution

38. Chiral separations

XX. (abstract number underlined) refers to HPTLC related publication or application using HPTLC materials

CAMAGBIBLIOGRAPHYSERVICE No.104�

1. Reviewsandbooks104001 TaraMCGLINCHEY*,P.A.RAFTER,FionaREGAN,D.GILLIAN,P.MCMAHON(*Depart-

mentofAgriculture,Fisheries&Food,CentralMeatControl,BackwestonLaboratoryComplex,YoungsCross,Celbridge,Co.,Kildare, Ireland):Areviewofanalyticalmethodsfor thedeter-minationofaminoglycosideandmacrolideresiduesinfoodmatrices.Anal.Chim.Acta624(1),1-15(2008).Aminoglycosidesandmacrolidesareimportantantibioticsforveterinarymedicineandarewidelyusedinthetreatmentofbacterialdisease,andasfeedadditivesforgrowthpromo-tion.AsaresulttheEuropeancommissionsetstrictcriteriaformonitoringresiduesandrequirestestingforlowlevelsofaminoglycosidesandmacrolidesinfoods.Thereforethedevelopmentoffast,reliable,andsensitivemethodsfortheextractionandsubsequentanalysisoftheseantibioticsisofgreatinterest.Thereviewdiscussesanalyticalmethodsforbothextractionanddeterminationofantibioticsinvariousfoodmatricesfocusingonthelast10years.Extractionandclean-upme-thodssuchasdeproteinizationandsolid-phaseextractionaredescribed,andvariousscreeningme-thodsincludingTLC,EI,CE,microbiologicalassays,andLCcombinedwithMSarereviewed.agricultural,food,analysis,HPTLC,

review 1,28

2. Fundamentals,theoryandgeneral104002 TatjanaDJAKOVIC-SEKULIC*,NadaPERISIC-JANJIC,EvgenijaDJURENDI(*Department

ofChemistry,FacultyofSciences,UniversityofNoviSad,TrgDositejaObradovia�,21000NoviSad,Serbia):Retentiondatafromreverse-phasehigh-performancethin-layerchromato-graphyincharacterizationofsomebis-salicylicacidderivatives.Biomed.Chromatogr.2�(8),881-887(2009).HPTLCinvestigationofsalicylicacidderivativesonRP-phasewithvariousmethanol-wateranddioxane-waterbinarymixturesinordertoestablishrelationshipsbetweenchromatographicdataandselectedphysico-chemicalparametersthatarerelatedtoADME(absorption,distribution,metabolismandelimination).AlinearcorrelationbetweenRMvaluesandthevolumefractionofmobilephasemodifierwasobserved.TheobtainedRM0valueswerecorrelatedwithlipophilicity,solubility,humanintestinalabsorption,plasma-proteinbinding,andblood-brainbarrierdata.

HPTLC,QSRR,lipophilicity 2

10400� L.KOMSTA*,K.SZTANKE,P.MACZKA,M.UCHEREK,R.SKIBINSKI,A.GUMIENIC-ZEK(*DepartmentofMedicinalChemistry,FacultyofPharmacy,MedicalUniversityofLublin,Jaczewskiego4,20-090Lublin,Poland;lukasz.komsta@am.lublin.pl):Determinationofthelipo-philicityoftwenty-sevenimidazo[2,1-c][1,2,4]triazinederivativeswithstrongbiologicalactivitybyreversed-phaseTLC.ComparisonwithresultsobtainedbyuseofcomputationalalgorithmsJ.PlanarChromatogr.22,�27-��1 (2009)TLCof27novel imidazo[2,1-c][1,2,4]triazinederi-vativestogetherwith12compoundswithknownliteraturelogPvalues(asreferencecalibrationdata) on RP-18 with methanol - water binary mobile phases containing different proportionsofmethanol inhorizontalchamberswithoutchambersaturation.DetectionunderUV254nm.Usingprincipal-componentanalysistheobtainedresultswerecomparedwithresultsfromninecomputationalmethods.

pharmaceuticalresearch,qualitativeidentification 2c

104004 T.SAMUEL*,A.MANIKANDAN,A.SINGH(*CGPSGCollegeofPharmacy,Peelamedu,Coimbatore,India):Standardisationofherbalmedicinebyhigh-performancethin-layerchro-matography.AbstractNo.992�,IHCB(2009).HPTLCofseveralherbalformulations(tabletsextractedwithmethanol)onsilicagelwithtoluene-ethylacetate19:1.Thefingerprintmethodwassuitableforcorrectidentificationandforroutinequalitycontroloftheherbalextracts.

pharmaceuticalresearchqualitycontrol,herbal,HPTLC 2a

104005 M. WAKSMUNDZKA-HAJNOS, D. MATOSIUK, A. PETRUCZYNIK, U. KIJKOWSKA-MURAK*(*MedicalUniversityofLublinDepartmentof InorganicChemistry20-081LublinPoland):DeterminationofthelipophilicityofselectedisoquinolinealkaloidsbyRP-TLC.ActaChromatographica 24 (4), 56�-57� (2008).TLC of nine alkaloids on RP-18 with mixtures of

CAMAGBIBLIOGRAPHYSERVICE No.1044

aqueousacetoneoraqueousdioxanewithvariousmobilephaseadditives (ammonia,diethyla-mine,or tetrabutylammoniumchloride) inorder tosuppress ionizationof thealkaloidsand/orreduceionicinteractionswithsurfacesilanolgroups.Ion-pairTLConRP-18withaqueousace-tonemixturesandvariousmobilephaseadditives(pentanesulfonicacid,octanesulfonicacid,ordi-(2-ethylhexyl)orthophosphoric acid). Investigation of relationships between RM values andmodifierconcentrationusinga linearsemilogarithmicequationforexperimentaldata tocalcu-latelipophilicityvaluesRMW(RMforpurewater),theslope,andtheinterceptwiththex-axis.Comparisonwithretentiondataofstandardswithknownlipophilicity(logP).

doping 2d,22

3. Generaltechniques104006 V.G.BEREZKIN*,N.Y.KULAKOVA,S.S.KHREBTOVA(*A.V.TopchievInstituteofPetro-

chemicalSynthesis,RussianAcademyofSciences,Leninskypr.29,Moscow,119991,Russia,berezkin@ips.ac.ru): Three-dimensional thin-layer chromatography on plates with open andclosedadsorption layers.J.PlanarChromatogr.22,�1�-�19(2009).Presentationof twodiffe-rentmethodsof three-dimensionalTLCusingplateswithopenandsealed(closed)adsorptionlayers.Inthesuggestedmethodthecomponentsofthetestdyemixtureinitiallymigrateinthefirst direction, then in the seconddirection (different from thefirst) and in the thirddirection(differentfromfirstandsecond).TLCofdyemixture1(crystalviolet,xylencyanol,neutralblue,bromothymoldarkblue,methanylyellow,acridineorange,indophenol,ariabelred,SudanblueII,SudanIV,dimethylaminoazobenzene)withethanol-aceticacid10:1(1D),acetone(2D),andto-luene(�D)andofmixture2(darkviolet,brightorange,yellow,darkred,violet)onsilicagelwithtetrahydrofurane-benzene9:1(1D),dichloromethane-benzene�:1(2D),andtoluene(�D).

comparisonofmethods �d

104007 X.LIU*,T.KUBO,H.DIAO,J.BENJAMAS,T.YONEMICHI,N.NISHI(*CollegeofMateri-alsandTextiles,KeyLaboratoryofAdvancedTextileMaterialsandManufacturingTechnology,MinistryofEducation,ZhejiangSci-TechUniversity,XiashaHigherEducationZone,Hangzhou�10018,China):DNA/polyvinyl alcohol interpenetratingpolymernetworkas stationaryphaseforthin-layerchromatography.Anal.Biochem.�9�(1),67-72(2009).ADNA/polyvinylalcoholinterpenetratingpolymernetworkwasproducedbycross-linkingpolyvinylalcoholwithglutar-aldehydeandsubsequentcross-linkingofDNAbyUVirradiation.ThepolymerwasthenusedtocoatthesurfaceofporoussilicaparticlesforTLC.ThreetypicalDNA-bindingcompoundsandeightaminoacidenantiomerswereusedasmodelchemicalstoinvestigatethechromatographicbehaviorofthemodifiedTLCphase.Bothclassesofchemicalsprovidedhighseparationeffici-ency.DNA-modifiedTLCphasescouldbeusedforvariousapplicationfields,includingefficacyevaluationofamedicine,toxicityassessmentofapollutantatthemolecularlevel,aswellasse-parationofenantiomersofdyes,aminoacids,peptides,proteins,nucleotides,anddrugs.

stationaryphase �b

104008 S. WANGTHONG*, I.TONSIRIPAKDEE, T. MONHAPHOL, R. NONTHABENJAWAN, S.PATTANAARGSONWANICHWECHARUNGRUANG(*DepartmentofChemistry,FacultyofScience, Chulalongkorn University, Payatai, Bangkok 10��0,Thailand): PostTLC developingtechniquefortyrosinaseinhibitordetection.Bio.Chromatogr.21(1),94-100(2008).ThemethodfordetectionoftyrosinaseinhibitingsubstancesinvolvessprayingoftheTLClayerwithtyrosi-naseandl-tyrosinesolutionssuccessively.Positiveresultsaredetectedaswhitespotsagainstabrownish-purplebackground.Themethodissuitableeitherasaquickscreeningmethodfortyro-sinaseinhibitordetectionorasaguidingprocedureforanisolationoftyrosinaseinhibitorsfrommixturesornaturalproductextracts.Thetechniqueissensitiveenoughforresultsinthepresenceof6ng/zoneglabridin.

review,postchromatographicderivatization �d

4. Specialtechniques104009 P.ABU-RABIE*,N.SPOONER(*PreClinicalDevelopmentDrugMetabolismandPharmaco-

kinetics,GlaxoSmithKlineResearchandDevelopment,ParkRoad,Ware,Hertfordshire,SG12

CAMAGBIBLIOGRAPHYSERVICE No.1045

ODP,UnitedKingdom;Paul.2.Abu-Rabie@gsk.com):Directquantitativebioanalysisofdrugsindriedbloodspotsamplesusingathin-layerchromatographymassspectrometerinterface.Anal.Chem.81,10275-10284(2009).DirectquantitativebioanalysisofdrugsfromdriedbloodspotsamplesusingaTLC-MSinterfacewithorwithoutHPLCseparation.Themethodgaveacceptab-lesensitivity,linearity,accuracy,andprecisiondataforbioanalyticalvalidations.Thedirecteluti-ontechniquewasshowntoincreaseassaysensitivityforarangeofanalytes.Investigationswereperformed to optimize extraction time, minimize sample-to-sample carry-over, and comparechromatographicperformance.Onthebasisofthispreliminaryassessment,ithasbeendemons-tratedthatthisTLC-MSinterfacehasthepotentialtobeaneffectivetoolforthedirectanalysisofdrugsindriedbloodsamplesatphysiologicallyrelevantconcentrations.

clinicalchemistryresearch 4e

104010 S.-C.CHENG(ChengSy-Chyi),M.Z.HUANG(HuangMin-Zong),J.SHIEA*(ShieaJentaie)(*NationalSunYat-SenUniversity-KaohsiungMedicalUniversityJointResearchCenter,Kaohsi-ung,804,Taiwan;jetea@mail.nsysu.edu-tw):Thin-layerchromatography/laser-inducedacousticdesorption/electrosprayionizationmassspectrometry.Anal.Chem.81,9274-9281(2009).TLCofdyestandards(FD&CGreenNo.�,FD&CRedNo.�,eriochromcyaninR),drugstandards(�,4-methylene-dioxy-N-methamphetamine, lysergicaciddiethylamide,flunitrazepam),andro-semaryessentialoilon1)RP-18with65%acetonecontaining1.5%formicacidand2)onsilicagelwithchloroform-methanol9:1.Rosemaryessentialoilwasalsoseparatedonsilicagelwithtoluene-ethylacetate9:1.DetectionunderUV254nmandindaylight.Thecombinationofla-ser-inducedacousticdesorptionandelectrosprayionizationmassspectrometry(LIAD/ESI/MS)canbeusedtorapidlycharacterizechemicalcompoundsseparatedonaTLCplate.

qualitativeidentification 4e

104011 N.GOTO-INOUE*,T.HAYASAKA,T.TAKI,TaniaVALDESGONZALEZ,M.SETOU(*De-partmentofMolecularAnatomy,HamamatsuUniversitySchoolofMedicine,Hamamatsu,Shi-zuoka4�1-�192,Japan):Anewlipidomicsapproachbythin-layerchromatography-blot-matrix-assistedlaserdesorption/ionizationimagingmassspectrometryforanalyzingdetailedpatternsofphospholipidmolecularspecies.J.Chromatogr.A1216(42),7096-7101(2009).PresentationofaTLC-blot-MALDI-IMSmethodwhichcombinesTLCandIMS(imagingmassspectrometry)foruseinlipidomics.Incomparisonwithcommonstainingmethodsthemethodallowshighlysensitivedetecionofwholelipidsandindividualmolecularspecies.Linearityforalllipidsrangedapproximatelyoveroneorderofmagnitude.Precision(%RSD)was

CAMAGBIBLIOGRAPHYSERVICE No.1046

11decompositionlevels)withtheoriginalnoisysignalandareferencesignalwhichwasdenoi-sed experimentallyby averaging64measurements.Thebest similarity to the reference signalwasobtainedwithfilters,howeverthesignalwasslightlyoversmoothed.Thewaveletshrinkagemethodgave lessdenoisedsignals.Therewasasignificant influenceof the thresholding tech-niqueanddecompositionlevel,andbestconditionswereatlevel2or�andsoftthresholding),whereaschangingofthemotherwaveletalmostdidnotchangetheresult.Thepresentedresultscanbeusedasgeneralrecommendationsfordenoisingdensitometricfingerprintsbeforeapply-ingfurtherchemometricalgorithms.Thebestchoiceswere:Savitzky-Golayfilterofappropriatewindowwidth(optimizedagainstautocorrelation)orwaveletshrinkagewithHaarwavelet,softthresholdingandhighdecompositionlevel.

HPTLC,quantitativeanalysis,qualitativeidentification,densitometry 4c

104014 F.SCHULTE, J.MAEDER,L.W.KROH,U.PANNE, JaninaKNEIPP* (*ChemistryDepart-ment,HumboldtUniversitätzuBerlin,Brook-Taylor-Strasse2,12489Berlin,Germany;janina.kneipp@chemie.hu-berlin.de):Characterizationofpollencarotenoidswithinsituandhigh-per-formancethin-layerchromatographysupportedresonantRamanspectroscopy.Anal.Chem.81,8426-84�� (2009). HPTLC of zeaxanthin, cryptoxanthin, beta-carotene, lutein and pollen ex-tractsonsilicagelwithtetrahydofuran-methylenechloride-n-hexanebyautomatedmultipledevelopment.Quantitativedeterminationbyabsorbancemeasurementat425nm,whichhastobeaccomplishedwithin5minafterdevelopmentduetothefastbleachingofthecarotenoidcolor.TheanalysisofcarotenoidsinpollenextractswasconfirmedbyresonanceRamandatameasureddirectlyontheHPTLCplates.

HPTLC,AMD,densitometry,quantitativeanalysis,biochemicalresearch4e,�0b

104015 M.SHARIATGORJI,Z.SPACIL,G.MADDALO,L.CARDENAS,L.ILAG*(*DepartmentofAnalyticalChemistry,StockholmUniversity,10691Stockholm,Sweden,Leopold.ilag@anchem.su.se):Matrix-freethinlayerchromatography/laserdesorptionionizationmassspectrometryforfacileseparationandidentificationofmedicinalalkaloids.RapidCommun.MassSpectrom.2�,�655-�660(2009).TLCofberberineandpalmatineinrootsofBerberisbarandanaonsilicagelwithbutanol-aceticacid-water14:�:4.DetectionunderUV�66nm.Bandswerecutoutforfurtheranalysisbylaserdesorptionionizationmassspectrometry.ThehRFvalueofberberineandpalmatinewas56and46,respectively.

herbal,qualitativeidentification 4e

104016 C.SIMOES-PIRES,B.HMICHA,A.MARSTON,K.HOSTETTMANN*(*LaboratoryofPhar-macognosyandPhytochemistry,UniversityofGeneva,1211Geneva4,Switzerland,kurt.hostett-mann@unige.ch):ATLCbioautographicmethodforthedetectionofalpha-andbeta-glucosidaseinhibitors inplant extracts.Phytochem.Anal. 20,511-515 (2009).Bioautographyof alpha-D-glucosidase (1) and beta-D-glucosidase (2) in buffer solution (sodium acetate 4.1 % in waterpH=7.5)sprayedontoasilicagelplate.Incubationatroomtemperaturefor60minfor(1)andat�7°Cfor20minfor(2).Fordetectionoftheactiveenzyme,solutionsof2-naphthyl-alpha-D-glucopyranosideor2-naphthyl-beta-D-glucopyranosideandFastBluesaltweremixedataratioof1:1for(1)or1:4for(2),andsprayedontotheplatetogiveapurplebackgroundcolorationafter2-5min.MethanolextractsoftheaerialpartsofTussilagofarfaraandUrticadioicaweretestedasenzymeinhibitorsandvisualizedaswhitespotsontheTLCplates.

pharmaceuticalresearch,herbal,qualitativeidentification,AMD,bioautography 4e

104017 G.STUBIGER,E.PITTENAUER,O.BELGACEM,P.REHULKA,K.WIDHALM,G.ALL-MAIER* (*InstituteofChemicalTechnologies andAnalytics,ViennaUniversityofTechnolo-gy,1060Vienna,Austria,guenter.allmaier@tuwien.ac.at):Analysisofhumanplasmalipidsandsoybeanlecithinbymeansofhigh-performancethin-layerchromatographyandmatrix-assistedlaserdesorption/ionizationmassspectrometry.RapidCommun.MassSpectrom.2�,2711-272�(2009).HPTLC in combinationwithmatrix-assisted laserdesorption/ionizationmass spectro-metry(MALDI-MS)wasusedfortheanalysisofcomplexlipidmixtures.Fortheseparationof

CAMAGBIBLIOGRAPHYSERVICE No.1047

lipidsone-dimensionalHPTLConsilicagelaluminumfoilwasusedwithatwo-phasemobilephase.ThecombinationwithMALDI-MSallowedtheidentificationof70distinctlipidspeciesandtheanalysisofevenminorlipidclassesfromonlyverysmallvolumesofhumanplasma(50µL).

pharmaceuticalresearch,clinicalchemistryresearch,foodanalysis,HPTLC,quantitativeanalysis 4e

5. Hydrocarbonsandhalogenderivatives104018 I.BELAI*,G.OROS,B.BORDAS(*PlantProtectionInstitute,HungarianAcademyofSciences,

1525Budapest,P.O.Box102,Hungary;ibel@nki.hu):Quantitativestructure-retentionrelation-shipand�Dmolecularmodelingstudiesintheunusualchromatographicbehavioroftriphenyl-methanederivativesinRPTLCsystems.J.PlanarChromatogr.22,255-26�(2009).TLCof25triphenylmethanederivativesusingparaffinoil-coatedsilicagelandacetone-watermixtures,inwhichtheacetonecontentvariedbetween40and70%inincrementsof10%.DualretentionbehaviorisobservedfortriphenylmethanederivativesinreversedphaseHPTLCwhenthecom-positionofacetone-watermobilephaseisvaried.Thephysicochemicalandmolecularpropertiesoftriphenylmethanederivativesleadtoanunusualretentionbehavior,whichwasinvestigatdbytraditionalquantitativestructure-retentionrelationshipmodelingandby�Dmolecularmodeling.Lipophilicitywasfoundtobethemostimportantmolecularpropertygoverningtheretentionoftriphenylmethanederivatives.

qualitativeidentification 5b

8. Substancescontainingheterocyclicoxygen104019 H.M.KURTBAY,I.KAYNAK,S.S.BOZKURT,M.MERDIVAN*(*DepartmentofChemistry,

DokuzEylulUniversity,FacultyofScienceandArts,�5160 Izmir,Turkey;melek.merdivan@deu.edu.tr):DensitometricHPTLCanalysisof the5-hydroxymethylfurfural contentofTurkishfruitwinesandvinegars.J.PlanarChromatogr.22,�6�-�66(2009).HPTLCof5-hydroxymethyl-furfuralinsevenTurkishfruitwinesandthreeTurkishvinegarsonsilcagelwithtoluene-ethylacetate-90%formicacid6:�:1inatwintroughchambersaturatedfor20min.Quantitativede-terminationbyabsorbancemeasurementat286nm.Thelimitofdetectionandquantificationwas0.05and0.1�ng/mL,respectively.

foodanalysis,toxicology,HPTLC,densitometry,quantitativeanalysis 8b

9. Oxocompounds,ethersandepoxides104020 PetraJAZBEC*,A.SMIDOVNIK,M.PUKLAVEC,M.KRIZMAN,J.SRIBAR,L.MILIVOJE-

VIC,M.PROSEK(*DepartmentofFoodChemistry,NationalIntituteofChemistry,Ljubljana,Slovenia;Petra.jazbec@ki.si):HPTLCandHPLC-MSquantificationofcoenzymeQ10andcho-lesterolinfractionatedchicken-breasttissue.J.PlanarChromatogr.22,�95-�98(2009).HPTLCofcoenzymeQ10,cholesterolandbiologicalextractsonsilicagelwithpetroleumether-diethylether-aceticacid85:15:1.Detectionbydippinginto5%phosphomolybdicacidinethanolfor10sfollowedbyheatingfor10minat110°C.Quantitativeevaluationinvisiblelight.

foodanalysis,HPTLC,quantitativeanalysis,densitometry,biochemicalresearch 9,20

10. Carbohydrates104021 T.BERNARDI,ElenaTAMBURINI*(*DepartmentofChemistry,UniversityofFerrara,ViaL.

Borsari46,44100Ferrara,Italy;tme@unife.it):AnHPTLC-AMDmethodforunderstandingthemetabolic behavior of microorganisms in the presence of mixed carbon sources.The case ofBifidobacterium adolescentis MB 2�9. J. Planar Chromatogr. 22, �21-�25 (2009). HPTLC ofglucose,fructose,galactose,lactose,raffinose,1-kestose,nystose,andfructosyl-nystoseondiolphasebyautomatedmultipledevelopmentwithacetonitrile-acetone-waterandacetonitrile-water.Preliminaryisocraticdevelopmentswereperformedat22-25°Cat65-75%relativehumi-dityinatwintroughchamber.Detectionbyvaporizationwith�7%hydochloricacidvaporfor�0minfollowedbydippingin4-aminobenzoicacid.Quantitativedeterminationbyfluorescencemeasurementat�1�nm.

HPTLC,densitometry,quantitativeanalysis,AMD,biochemicalresearch 10a

CAMAGBIBLIOGRAPHYSERVICE No.1048

104022 J. STROKA*, I. DONCHEVA, B. SPANGENBERG (*European Commission Joint ResearchCentre,InstituteforReferenceMaterialsandMeasurements,FoodSafetyandQualityUnit,Re-tieseweg111,2440Geel,Belgium; joerg.stroka@ec.europa.eu):Determinationofsucralose insoftdrinksbyhigh-performancethin-layerchromatography:Interlaboratorystudy.J.AOACInt.92,115�-1159 (2009).HPTLCofsucraloseonaminophasewithacetonitrile -water4:1 inahorizontalorstandarddevelopmentchamberwithoutchambersaturation.Fordetectiontheplatewasheatedat190°Cfor20min,eitherinadryingovenoronatemperature-controlledheatingplate.Quantitativedeterminationbyabsorbanceandfluorescencemeasurementat254nm.Theresultsoftheinterlaboratorycomparisonshowgoodprecisioncharacteristics.Thefluorescencemeasurementsofthesucralosederivativesindicatedbettermethodperformance,comparedwithabsorbancemeasurementsintheUV.

foodanalysis,qualitycontrol,HPTLC,quantitativeanalysis,densitometry 10a

11. Organicacidsandlipids10402� RituARORA*,B.SINGH,R.SINGH,C.KATIYAR(*GuruNanakDevUniversity,Amritsar,

Punjab,India):ValidatedHPTLCmethodforthedeterminationofcinnamicacidincrudeplantmaterials,herbalextractsandpharmaceuticaldosageformscontainingCinnamomumcassia.60thIndianPharmaceuticalCongressPA-214(2008).HPTLCofcinnamicacid(inplantrawmaterial,herbalextractsandpharmaceuticaldosageforms)onsilicagelwithchloroform-methanol4:1inasaturatedtwintroughchamberatroomtemperature(25°C).Quantitativedeterminationbyabsorbancemeasurementat277nm.ThehRFvalueforcinnamicacidwas50.Themethodwaslinearintherangeof700-1400ng/spot.

pharmaceuticalresearch,herbal,HPTLC,densitometry,quantitativeanalysis 11a

104024 F.HASAN*,R.KHAR,F.AHMAD,M.ALI,M.RAZA(*Dept.ofPharmaceutics,JamiaHam-dard, Hamdard Nagar, New Delhi, India): Development of novel high-performance thin-layerchromatographymethodforestimationoflipidineggoil.AbstractNo.F-282,61st(2009).HPT-LCoflipidsonsilicagelinasaturatedtwintroughchamberwithcarbontetrachloride-methanol-aceticacid270:�0:11atroomtemperature(25°C).Quantitativedeterminationbyfluorescencemeasurementat�66nm.ThehRFvalueofcholesterolwas�5.Thecalibrationcurveshowedgoodlinearrelationshipwithr2=0.999intherangeof100-600ng/spot(viapeakarea).

pharmaceuticalresearch,qualitycontrol,HPTLC,quantitativeanalysis 11c

104025 P.HAZAM*,D.SARKAR,B.DEY,S.DAS(*HimalayanPharmacy Institute,Dept.ofPhar-macognosy,Majhotar,Sikkim,India:Ahigh-performancethin-layerchromatographic(HPTLC)method for theestimationof rosmarinicacid fromSalviaofficinalis (sage).60th IndianPhar-maceuticalCongressPG-256(2008).HPTLCof rosmarinicacid inSalviaofficinalisonsilicagelwith toluene -ethylacetate - formicacid5:4:1.Quantitativedeterminationbyabsorbancemeasurementat�28nm.Linearitywas0.1-1.0ng/mL,recoverywas99.4%.ThemethodwasfoundsuitableforroutinequalitycontroloftheSalviaofficinalisrawmaterial.

herbal,environmental,densitometry,HPTLC,quantitativeanalysis 11a

104026 Y. KAWAI*, M. MIYOSHI, J. MOON, J. TERAO (*Department of Food Science, GraduateSchool of Nutrition and Biosciences,The University ofTokushima,Tokushima 770-850�, Ja-pan): Detection of cholesteryl ester hydroperoxide isomers using gas chromatography-massspectrometrycombinedwiththin-layerchromatographyblotting.Anal.Biochem.�60(1),1�0-1�7 (2007). Determination of cholesteryl ester hydroperoxides, especially cholesteryl linole-atehydroperoxideisomers,bycombinationofTLCblottingwithdiphenyl-1-pyrenylphosphinefluorescentdetection(DPPP-TLCblotting)andGC-electronionization-MS(GC-EI-MS).AfterDPPP-TLCblottingofcholesterylesterhydroperoxidesfluorescentzoneswereobtianedwhichwereextractedandderivatizedbyhydrogenation,transmethylation,andtrimethylsilylation.Theresultingmethylester/trimethylsilyletherderivativesofhydroxyoctadecenoicacidwerethenana-lyzedbyGC-EI-MSusingselectedionmonitoringofisomer-specificfragmentionsoriginatingfromthealpha-cleavageofthetrimethylsilyloxylgroup.

CAMAGBIBLIOGRAPHYSERVICE No.1049

agricultural,clinicalroutineanalysis,postchromatographicderivatization,qualitativeidentification,quantitativeanalysis 11

104027 H.LI(LiHaixing)*,T.QIU(QiuTing),Y.CAO(CaoYusheng),J.YANG(YangJiyan),Z.HU-ANG(HuangZhibing)(*Sino-GermanJointResearchInstitute,NanchangUniversity,Nanchang��0047,China):Pre-stainingpaperchromatographymethodforquantificationofgamma-amino-butyricacid.J.Chromatogr.A1216(25),5057-5060(2009).Paperchromatographyofgamma-aminobutyric acid.The method consists of application, separation and detection and is clean,rapid,inexpensiveandreproduciblecomparedtotheroutinepaperchromatography.Thederiva-tizationprocedurewithninhydrinreagentwasoptimizedregardingreagentconcentration,deri-vatizationtemperatureandtimeandCu2+concentration.Quantificationofgamma-aminobutyricacidbycombinationofwithvisspectrophotometry.Thelimitofdetectionwas0.05mg/mLandthelinearrangewasfrom0.5to20.0mg/mL.Thedeterminationcoefficientwasr2=0.998.Themethodwasaccurate(%RSD<2.6%),andrecoverieswere102.7-10�.9%.

qualitycontrol,traditionalmedicine,pharmaceuticalresearch,quantitativeanalysis,qualitativeidentification,paperchromatography 11a

104028 N. MANJU*,A. BINDU, N.ALEYKUTTY, J. SAJAN (*Department of Pharmaceutical Sci-ences,CheruvandoorCampus,Ettumanoor,Kottayam,Kerala,India):DevelopmentofHPTLCmethod forquantificationofgallic acid from the fruitsofPhyllanthusemblicaL.60th IndianPharmaceuticalCongressPG-265(2008).HPTLCofgallicacidintheethylacetatefractionoffruitsofPhyllanthusemblicaonsilicagelwithtoluene-ethylacetate-formicacid-methanol�0:�0:8:2.Detectionandquantitativedeterminationofgallicacidbyabsorbancemeasurementat280nm.TheproposedHPTLCmethodprovidedagoodresolutionofgallicacidfromotherconstituentspresentintheethylacetatefractionoffruitsofPhyllanthusemblicaandcanbeusedforthequantificationofgallicacid.

herbal,HPTLC,densitometry,quantitativeanalysis 11a

104029 D.MUKHERJEE*,T.BARMAN,S.RAJA,P.MUKHERJEE(*SchoolofNaturalProductStu-dies,JadavpurUniversity,Kolkata7000�2,India):EstimationofbetulinicacidinNelumbonu-cifera(Nymphaceae)rhizomeandseedextractbyvalidatedHPTLCmethod.AbstractNo.9192,IHCB(2009).HPTLCofbetulinicacidinhydroalcoholicextractsofNelumbonuciferarhizomeandseed,onsilicagelwithchloroform-methanol-formicacid49:1:1.Detectionbysprayingwithanisaldehydereagent.Quantitativedeterminationbyabsorbancemeasurementat420nm.Themethodwaslinearintherangeof2-10ng/spot,recoverywas98.1-98.4%.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis,postchromatographicderivatization 11a

1040�0 B.NIMAVAT*,D.MOVALIA,S.MISHRA,H.TANK(*S.J.ThakkarPharmacyCollege,Sau-rashtraUniversity,Rajkot,Gujarat,India):DevelopmentofvalidatedHPTLCmethodforquan-titative estimation of oleanolic acid as marker in total methanolic extract of fruits of Randiadumetorumlam.60thIndianPharmaceuticalCongressPA-217(2008).HPTLCofoleanolicacidintotalmethanolicextractoffruitsofRandiadumetorumlam.onsilicagelwithtoluene-ethylacetate-glacialaceticacid70:�0:1inatwintroughchambersaturatedfor10min.Detectionbytreatmentwith10%sulphuricacidinmethanol,followedbyheatingat110°Candimmediatedensitometricevaluation.Quantitativedeterminationbyabsorbancemeasurementat540nm.Themethodwaslinearintherangeof50-500ng/spot.Recoverywasintherangeof99.4-100.8%.

pharmaceuticalresearch,traditionalmedicine,herbal,HPTLC,quantitativeanalysis 11a

1040�1 P.PATEL*,R.SHAH,S.PATEL,UnnatiSHAH(*PharmanzaHerbalPvt.Ltd.,PlotNo.214,Kania�884�5,Gujarat,India;andLachooMemorialCollegeofScience&Technology,Jodhpur,India):Methoddevelopmentandvalidationfortheestimationof(-)hydroxycitricacidinfruitsofGarciniagummiguttaD.byHPTLC.AbstractNo.9191,IHCB(2009).HPTLCof(-)hydroxy

CAMAGBIBLIOGRAPHYSERVICE No.10410

citricacid(themainconstituentofGarciniagummiguttafruits)onsilicagelwithn-propanol-water - glacial acetic acid 50:50:1. Quantitative determination by absorbance measurement at210nm.ThehRFvaluewas46.Themethodwaslinearintherangeof100-1000ng/spot,recove-rywas99.8-100.9%.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis 11a

1040�2 B.RAJ*,SalmaKHANAM,L.JOSEPHINE(*Dept.ofPharmacognosy,DayanandSagarCollegeofPharmacy,Bangalore560078,India,bincyraj@yahoo.com):HPTLCmethodforestimationofursolicacid inOcimumsanctumextract.AsianJ.ofChem.21(9),6999-7004(2009).HPTLCofursolicacidinmethanolicandaqueousextractsofOcimumsanctum(Tulsi)onsilicagelwithtoluene-ethylacetate-aceticacid55:45:2withchambersaturation.DetectionbytreatmentwithLiebermannBurchard‘sreagent.Quantitativedeterminationbyabsorbancemeasurementat550nm.Themethodwaslinearintherangeof100-400ng/band.Theamountofursolicacidinaque-ousandmethanolicextractswasintherangeof0.2and0.4%.Samplescollectedfromdifferentgeographicalregionswerecompared,samplesfromKeralacontainedthehighestlevelsofursolicacid.

pharmaceuticalresearch,qualitycontrol,densitometry,HPTLC,quantitativeanalysis 11a

1040�� B.RAJ*,SalmaKHANAM,S.JOHN,J.JENITA,AyeshaSIDDIQUA(*Dept.ofPharmacogno-sy, Dayananda Sagar College of Pharmacy, Kumaraswamy Layout, Bangalore 560078, India):ComparativeHPTLCanalysisofoleanolicacidinOcimumsanctumcollectedfromdifferentge-ographicalsources.AbstractNo.9226,IHCB(2009).HPTLCofoleanolicacid(inextractsofOcimumsanctumcollectedfromdifferentgeographicalsources)onsilicagelwithtoluene-ethylacetate-glacialaceticacid55:45:2.DetectionbysprayingwithLiebermann-Burchard‘sreagent.Quantitativedeterminationbyabsorbancemeasurementat600nm.Linearitywas in the rangeof 1-4 µg, recovery was 100.4-102.1 %. Hydro alcoholic extracts of the plant contained highamountsofoleanolicacid,maximumcontentswerefoundinplantscollectedintheKeralaregion.

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1040�4 M.SAJEWICZ,D.KRONENBACH,M.GONTARSKA,M.WRÓBEL,R.PIETKA,TeresaKO-WALSKA*(*InstituteofChemistry,SilesianUniversity,9SzkolnaStreet,40-006Katowice,Po-land;kowalska@us.edu.pl):TLCinasearchforstructurallimitationsofspontaneousoscillatoryin-vitrochiralconversion.Alpha-hydroxybutyricandmandelicacids.J.PlanarChromatogr.22,241-248(2009).TLCofalpha-hydroxybutyricacidsandmandelicacidonsilicagel,prewashedwithmethanol-water9:1andimpregnatedbydippingfor2sin0.05g/Laqueouscopperace-tatesolution,withdioxane-water9:1at22+/-2°C.Quantitativedeterminationbyabsorbancemeasurementduring16daysat�26nm.Spontaneousoscillatoryin-vitrochiralconversionwasobservedforalpha-substitutedpropionicacidsaswellaschiralcarboxylicacidswith twoandfourcarbonatoms.

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13. Steroids1040�5 R.XIA(XiaRui)*,SH.DONG(DongShuying),B.CHE(CheBaoquan)(*BeijingMunicip.Inst.

DrugCont.,Beijing1000�5,China):(RapididentificationofglucocorticoidinChinesetraditi-onalmedicinalformulationsbythin-layerchromatography)(Chinese).ChineseJ.Pharm.Anal.28(�),470-471(2008).TLCofglucocorticoidinTCMformulationsextractedwithchloroform-methanol9:1onsilicagelwithdichloromethane-diethylether-methanol-water�85:60:15:2.Detectionby sprayingwith a solutionof tetrazoliumblue chloride.Successful separation andidentificationoffiveglucocorticoids.

doping,pharmaceuticalresearch,traditionalmedicine,qualitycontrol,quantitativeanalysis,qualitativeidentification 1�

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1040�6 B.YUAN(YuanBaoqiang)*,L.Yang(YangLahu)(*FuzhouMunicip.Inst.DrugCont.,Fuzhou,Fujian�50001,China):(Analysisofdexamethasoneacetateandtherelatedcompoundsintheta-blets)(Chinese).ChineseJ.Pharm.Anal.27(�),412-41�(2007).TLCofdexamethasoneacetateonsilicagelwithdichloromethane-methanol9:1.DetectionunderUV254nm.

pharmaceuticalresearch,qualitycontrol,qualitativeidentification,quantitativeanalysis 1�

15. Terpenesandothervolatileplantingredients1040�7 B.CHENGAIAH*,B.PRATAP,M.ALAGUSUNDARAM,M.RUTHU,V.SAROVARREDDY

(*AnnamacharyaCollegeofPharmacy,Rajampet,Kadapa,A.P.,India):IdentificationofterpenesinstemofOcimumbasilicumLinnbyHPTLCtechnique.60thIndianPharmaceuticalCongressPA-221(2008).HPTLCof terpenesinstemofOcimumbasilicumonsilicagelwithtoluene-ethylacetate19:1.Evaluationof5spotsunderUV254nmandundervisiblelightaftertreatmentwithanisaldehydereagentfollowedbyheatingat100°Cfor5min:borneol(yellow,hRF24),menthol(red,hRF27),eugenol(blue,hRF50),thymol(violet,hRF57),safrole(blue,hRF9�).

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17. Amines,amidesandrelatednitrogencompounds1040�8 A.ALPMANN,GertrudMORLOCK*(*UniversityofHohenheim,InstituteofFoodChemeistry,

Garbenstrasse28,70599Stuttgart,Germany;gmorlock@uni-hohenheim.de):Rapidandcost-ef-fectivedeterminationofacrylamideincoffeebyplanarchromatographyandfluorescencedetec-tionafterderivatizationwithdansulfinicacid.J.AOACInt.92,725-729(2009).HPTLCofacryl-amideextracted fromcoffeesamplesonsilicagelwithethylacetate - tert.butylmethylether4:1inatwintroughchamberorautomaticdevelopingchamber.Pre-chromatographicinsitude-rivatizationoftheextracts(appliedasarea)byoversprayingwithdansulfinicacidproducedthefluorescentdansylpropanamideband.Quantitativedeterminationbyfluorescencemeasurementat254/>400nm.Thelimitofquantificationwas48µg/kg.Thelinearityoverthewholeprocedureshoweddeterminationcoefficientsbetween0.9995and0.9825(n=6).Thewithin-runprecision(%RSD,n=6)ofthechromatographicmethodwas�%.Commercialcoffeesamplesanalyzedshowedacrylamidecontentsbetween52and191µg/kg,whichwasincorrelationwithamountsreportedinpublications.

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18. Aminoacidsandpeptides,chemicalstructureofproteins1040�9 J.D.VASTA,M.CICCHI, J.SHERMA*,B.FRIED(*LafayetteCollege,DepartmentofChe-

mistry,EastonPA18042-1782USA):Evaluationofthin-layerchromatographysystemsforana-lysisofaminoacids incomplexmixtures.ActaChromatographica21 (1),29-�8 (2009).Eva-luationofdifferentTLCsystemsforanalysisof21aminoacidsinbiologicaltissuesandfluids.Detectionbyderivatizationwithninhydrinreagent,anddeterminationofRFvaluesbyslit-scan-ningdensitometry.Thefivemostsuitablesystemswerecelluloseandsilicagelplatesdevelopedwitheither2-butanol-pyridine-aceticacid-water�9:�4:10:26or2-butanol-pyridine-25%ammonia-water�9:�4:10:26,andionexchangeplatesdevelopedwithcitratebufferofpH�.�.Detection with ninhydrin allowed the identification of all amino acids except for leucine andisoleucineincomplexmixtures.Quantificationispossibleaswelliftheaminoacidofinterestiswellseparatedfromadjacentcomponentsofthemixture.ThemethodisillustratedwithexamplechromatogramsoncelluloseHPTLC layer showing the identificationand separationof aminoacidsinsnailtissuesamples.

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104040 M.VEGA*, M.ARANDA (*University of Concepcion, Faculty of Pharmacy, Department ofFoodScience,NutritionandDietetic,BarrioUniversitarios/nCasilla2�7,PO40�-0249Con-cepcion,Chile;mveha@udec.cl):Determinationofavailablelysinebyplanarchromatography:Ausefultoolforproteinqualityevaluationinfishfeed.J.AOACInt.92,699-702(2009).HPTLCof a dinitrophenyl-lysine derivative (produced by incubation with 1-fluoro-2,4-dinitrobenzeneandhydolyzationwithhydrochloricacid)onsilicagel (prewashedwithmethanol)withn-pro-

CAMAGBIBLIOGRAPHYSERVICE No.10412

panol-25%ammonia7:�inatwintroughchamber.Quantitativedeterminationbyabsorbancemeasurementat�60nm.Themethodwaslinear(r2=0.9991)intherangefrom12.5to125.0ng/band.Repeatability(%RSD)andintermediateprecision(%RSD)inmatrixwere0.8%and�.6%,respectively.Recoveriesofspikedsamplesattwolevelsrangedfrom72to85%withRSDfrom�to8%.Thismethodisareliable,highthroughputandlowcostanalyticalmethodforthesalmonfeedindustry.

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20. Enzymes104020 PetraJAZBECetal.,seesection9

22. Alkaloids104041 K.DHALWAL*,V.SHINDE,K.MAHADIK(*Dept.ofPharmacognosyandPhytochemistry,

PoonaCollegeofPharmacy,BharathiVidyapeethUniversity,Erandwane,Pune4110�8,India):Effective and sensitivemethods for quantitative analysis of alkaloids in sida species byusingHPLCandHPTLC.AbstractNo.9402,IHCB(2009).HPLCandHPTLCmethodsweredevelo-pedforthesimultaneousestimationofvasicineandvasicinoneinSidacordifoliaandSidaacutaroots.HPTLCofvasicineandvasicinoneonsilicagelwithethylacetate-methanol-ammonia40:10:1.Quantitativedeterminationbyabsorbancemeasurementat�00nm.Linearitywas�20-960ng/spot (vasicine) and80-400ng/spot (vasicinone).LinearitybyHPLCwas4-20µg/mL.TheHPTLCmethodwasmoresuitablebecauseofhighthroughputandlowanalysistime.

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104042 Danuta RAJ*, A. KOKOTKIEWICZ, M. LUCZKIEWICZ (*Department of Pharmacognosy,WroclawMedicalUniversity,pl.Nankiera1,50-140Wroclaw,Poland;dankaraj@wp.pl):Densi-tometricHPTLCanalysisofindolizidinealkaloidsintheherbandin-vitrocultureofSecurinegasuffruticosa. J. Planar Chromatogr. 22, �71-�76 (2009). HPTLC of indolizidine alkaloids andextractsonsilicagelandRP-18(bothprewashedwithchloroform-methanol1:1)with11mobilephasesinahorizontalchamberwithoutchambersaturation.Thebestresolutionwasachievedonsilicagelwithchloroform-methanol20:1.DetectionunderUV254nmandaftersprayingwithDragendorffreagent.Quantitativedeterminationofsecurinineandallosecurininebyabsorbancemeasurementat254nm.Thelimitofdetectionandquantificationwas11and�6ng/zoneforse-curinineand12and41ng/zoneforallosecurinine,respectively.

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10404� H.WIEDENFELD*,G.HOESCH,E.ROEDER,TH.DINGERMANN(*PharmazeutischesIns-titutderUniversität,Ander Immenburg4,5�121Bonn,Germany;wiedenfeld@uni-bonn.de):LycopsamineandcumambrinB fromEupatoriummaculatum.Pharmazie64,415-416 (2009).TLCofthepyrrolizidinealkaloidlycopsamineandtheguaianolidecumambrinBonsilicagelwithdichloromethane-methanol-25%ammonia85:14:1.DetectionseeA.R.Mattocks,Detec-tionofpyrrolizidinealkaloidsonthin-layerchromatograms,J.Chromatogr.27,505-508(1967).

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104005 M.WAKSMUNDZKA-HAJNOSetal.,seesection2

104044 L.ZHANG(ZhangLu)*,H.LI(LiHongyu),Y.WEI(WeiYuhui)(*StateKeyLabofMinist.Educ.ofDrought&GrassplotZoology,Coll.LifeSci.,LanzhouUniv.,Lanzhou7�0000,China):(Analysis of the alkaloids in the seedsofSophoramoorcroftiana (Benth.)Baker byTLCandHPLC)(Chinese).ChineseJ.Pharm.Anal.28(7),1071-1074(2008).TLCofthealkaloidsma-trine,oxymatrine,sophocarpine,sophoridine,cytosinetheinseedextractsofSophoramoorcrof-tianaonsilicagelwithchloroform-methanol-ammonia50:6:1.DetectionunderUV254nm.

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Comparisonwith reference standards showed that extracts containedmatrine, oxymatrine, so-phocarpine,sophoridine,andcytosine.

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27. Vitaminsandvariousgrowthregulators104045 A.MOHAMMAD*,A.ZEHRA(*AligarhMuslimUniversity,AnalyticalResearchLaboratory,

DepartmentofAppliedChemistry,FacultyofEngineeringandTechnology,Aligarh,India):Spe-cificseparationofthiaminefromhydrophilicvitaminswithaqueousdioxaneonprecoatedsilicaTLCplates.ActaChromatographica20(4),6�7-642(2008).TLCofthiaminehydrochloridefromriboflavin, nicotinic acid, calcium D-pantothenate, pyridoxine hydrochloride, cyanocobalamin,andascorbicacidonsilicagelwithdioxane-water1:1.DetectionunderUVlight.Examinationoftheeffectofimpurities(metalcationsandinorganicanions)onthechromatographyofthiaminehydrochloride.Thedetectionlimitforthiaminehydrochloridewas90ng/spotand%RSDofthia-minehydrochloridewas14.9%(n=5).

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104046 A.MOHAMMAD*,A.ZEHRA(*AnalyticalResearchLaboratory,DepartmentofAppliedChe-mistry,FacultyofEngineeringandTechnology,AligarhMuslimUniversity,Aligarh202002,In-dia;mohammadali4u@rediffmail.com):Simultaneousseparationandidentificationofcyanoco-balamin,thiamine,andascorbicacidonpolyoxyethylenesorbitanmonooleate-impregnatedsilicalayerswithwaterasmobilephase.J.PlanarChromatogr.22,429-4��(2009).TLCofthewater-solublevitaminscyanocobalamine,thiamine,andascorbicacidonsilicagel(impregnatedwitha2%solutionofthenon-ionicsurfactantTween80)withdoubledistilledwateringlassjarssatu-ratedfor�0minat�0+/-2°C.Detectionofallsubstancesexceptfolicacidandcyanocobalaminbyexposuretoiodinevaporandevaluationindaylight.

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104047 M.SUE-CHU,S.KRISTENSEN,H.H.TONNESEN*(*UniversityofOslo,SchoolofPharma-cy,DepartmentofPharmaceutics,P.O.Box1068,Blindern,0�16Oslo,Norway;h.h.tonnesen@farmasi.nio.no):Photoinducedcolorchangesintwodifferentqualitiesofriboflavininthesolidstateandvarioustabletformulations.Photoreactivityofbiologicallyactivecompounds.Pharma-zie64,428-4�5(2009).TLCofriboflavinandlumichrome(7,8-dimethylbenzo[g]pteridine-2,4-(1H,�H)-dione)onsilicagelwithaceticacid-acetone-methanol-benzene1:1:4:14DetectionundervisiblelightandUV254and�66nm.

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28. Antibiotics,Mycotoxins104242 R.BHUSHANetal.,seesection�8

104048 U.HUBICKA,J.KRZEK*,H.WOLTYNSKA,B.STACHAZ(*CollegiumMedicumofJagiel-lonianUniversity,DepartmentofInorganicandAnalyticalChemistry,Medyczna9,�0-688Kra-kow,Poland;jankrzek@cm-uj.krakow.pl):Simultaneousidentificationandquantitativedetermi-nation of selected aminoglycoside antibiotics by thin-layer chromatography and densitometry.J.AOACInt.92,1068-1075(2009).TLCandHPTLCofsixantibiotics(amikacin,gentamicin,kanamycin,neomycin,netilmicin,andtobramycin)inpharmaceuticalpreparationsonsilicagelwithmethanol-25%ammonia-chloroform�:2:1.Detectionbyderivatizationwith0.2%etha-nolicninhydrinreagent.Quantitativedeterminationbyabsorbancemeasurementat500nm.Thelimitofdetectionandquantificationwas250and500ng/zoneforamikacin,500and1000ng/zoneforkanamycin,480and800ng/zoneforneomycin,�80and6�0ng/zonefornetilmycin,480and800ng/zonefortobramycinand1000and1650ng/zoneforgentamicin.Precisionwasgoodwith%RSDof0.�-0.6%.

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CAMAGBIBLIOGRAPHYSERVICE No.10414

104049 S.JOSHI*,A.SHARMA,M.S.M.RAWAT,C.DHIMAN(*DepartmentofChemistry,K.L.D.A.V.(P.G.)College,Roorkee-247667.India;shajoshi@yahoo.com):Developmentofconditionsfor rapid thin-layerchromatographyofbeta-lactamantibiotics. J.PlanarChromatogr.22,4�5-4�7(2009).TLCofpenicillins(benzylpenicillin,ampicillin,andamoxicillin)andcephalosporins(cephalexin,cefoperazone,ceftriaxone,cefixime,andcefadroxil)inpowderextractsonsilicagel(impregnatedwith0.2%ammoniumchloride)withpropanol-aceticacid4:1andbutanol-ace-ticacid-water4:1:2.DetectionunderUVlightat�65nm.

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104001 TaraMCGLINCHEYetal.,seesection1

104050 P.N.RANJANE*,S.V.GANDHI,S.S.KADUKAR,K.G.BOTHARA,(*DepartmentofPharma-ceuticalAnalysis,A.I.S.S.M.S.CollegeofPharmacy,KennedyRoad,NearR.T.O.,Pune411001,India): HPTLC determination of cefuroxime axetil and ornidazole in combined tablet dosageform.J.Chromatogr.Sci.48(1),26-28(2010).HPTLCofcefuroximeaxetilandornidazoleincombinedtabletdosageformonsilicagelwithtoluene-n-butanol-triethylamine17:4:1.ThehRFvalueofornidazolewas51andofcefuroximeaxetil67.Quantificationbydensitometryat285nm.Linearitywasbetween100and500ng/bandforbothcefuroximeaxetilandornidazole.Themethodwasusedfortheassayofthecompoundsinpharmaceuticalformulations.Thecon-tentofcefuroximeaxetilwas102.4%andofornidazole101.0%.

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104051 A.R.ROTE*,S.P.PINGLE*(*DepartmentofPharmaceuticalChemistry,M.G.V.‘sPharmacyCollege,Panchavati (PuneUniversity)Mumbai,Agra Road,Nashik42200�,Maharashtra, In-dia):Reversephase-HPLCandHPTLCmethodsfordeterminationofgemifloxacinmesylateinhumanplasma.J.Chromatogr.B877(29),�719-�72�(2009).HPTLCofgemifloxacinmesylateinhumanplasma,extractedwithchloroform-aceticacid59:1,onsilicagelwithethylacetate-methanol-ammonia8:4:�.ThehRFvalueofgemifloxacinmesylatewas��.Quantificationbydensitometryat254nm.Thecalibrationcurvewasestablishedintherangeof50to600ng/spot.Recoveryofgemifloxacinmesylatewasbetween80.0and86.2%.Thestabilityofgemifloxacinmesylateinplasmawasconfirmedwithsamplessubmittedtothreecyclesoffreeze-thawingat

CAMAGBIBLIOGRAPHYSERVICE No.10415

QualityUnit,Retieseweg,2440Geel,Belgium,christoph.von-holst@ec.europa.eu):Validationofananalyticalmethodforthedeterminationofspiramycin,virginiamycin,andtylosininfeeding-stuffsby thin-layer chromatographyandbio-autobiography.FoodAddit.Contam.24,�51-�59(2007). Inter-laboratoryvalidationof the analyticalmethod (published in theSIMBAG-FEEDreport4.6)basedonTLCcoupledtobio-autographyforthedetectionoftylosin,spiramycinandvirginiamycininfeeding-stuffsforpoultry,pig,cattleandcalf.Thedetectionlimitofspiramycinwas2mg/kgandthemethodhasatargetconcentrationof1mg/kgfortylosinandvirginiamycin.ThemethodshowedhighspecificityandoffersthepossibilityforscreeningbeforeLC/MSanalysis.

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104054 L.YANG (Yang Lihong)*, CH. HU (Hu Changqin), W. LIU (Liu Wenying) (*China Pharm.Univ., Nanjing 210009, China): (Determination of gentamycin and the related compounds bythin-layerchromatography)(Chinese).ChineseJ.Pharm.Anal.26(2),221-224(2006).HPTLCofgentamycinandrelatedcompoundsonsilicagelwithchloroform-methanol-25%ammonia5:7:6.Themaincompoundiswellseparatedfromtheimpurities.Quantificationbydensitometryat485nm.Linearitywasbetween4.0-40ng/spot(r2=0.99)andthelimitofdetectionwasatthelownglevel.

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29. Pesticidesandotheragrochemicals104055 V.R.CHANDEGAONKAR,D.B.SHINDE,D.V.MANE* (*DepartmentofChemistry,Chhat-

rapatiShivajiCollege,Omerga,(MS)41�606India;manedv.2007@rediffmail.com):Thin-layerchromatographic detection and identificationof the insecticide imidacloprid in biologicalma-terials.J.PlanarChromatogr.22,459-460(2009).TLCof imidacloprid(1-[(6-chloro-�-pyridi-nylmethyl)]-4,5-dihydro-N-nitro-1H-imidazol-2-amine)andbiologicalextractsonsilicagelwithchloroform-acetone7:�orhexane-acetone-ethanol8:1:1withchambersaturation.Detectionbysprayingwith5%dimethylaminobenzaldehydeinhydrochloricacid,followedbyheatingat100°Cfor10min.Imidaclopridwasdetectedasapinkzoneundervisiblelight.

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104056 V.R.CHANDEGAONKAR,J.N.SANGSHETTI,D.B.SHINDE,D.V.MANE*(*DepartmentofChemistry,ChhatrapatiShivajiCollege,Omerga(MS)4�1606,India;manedv.2007@rediffmail.com):Anewchromogenic spray reagent fordetectionand identificationofmonocrotophos. J.PlanarChromatogr.22,457-458(2009).TLCofmonocrotophosandbiologicalextracts,dime-thoate,endosulfan,carbaryl,andcypermethrinonsilicagelwithchloroform-acetone7:�withchambersaturation.Detectionbysprayingwith5%sodiumhydroxidesolutionfollowedby5%benzilreagent(5gbenzilin100mLacetone)andheatingat100°Cfor10min.Monocrotophoswasdetectedasapinkzoneindaylight.

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104057 W.SCHWACK*,T.ZEISLER,C.STIEFEL(*UniversityofHohenheim,InstituteofFoodChe-mistry,Garbenstrasse28,70599Stuttgart,Germany;wschwack@uni-hohenheim.de):Determi-nationofdialkylphosphates asbreakdownproductsoforganophosphorus insecticides in fruitjuicesbyHPTLCwithfluorescencedetection.J.AOACInt.92,691-697(2009).HPTLCofdi-alkylphosphatestandards(dimethylphosphate,diethylphosphate,dimethylthiophosphate,diet-hylthiophosphateanddibutylphosphateasinternalstandard)onaminophase,prewashedwithmethanol,withdichloromethane in a twin troughchamber.Quantitativedeterminationbyflu-orescencemeasurement at �66/>400nm.The limitofquantificationwasbetween0.8 and1.4ng/zone.Fluorescenceenhancementwasachievedbydippingtheplateintoa50%solutionofparaffinoilinn-hexane,increasingthesensitivityandresultinginanLOQof0.5-0.6ng/zone.

agricultural,toxicology,qualitycontrol,foodanalysis,HPTLC,densitometry,quantitativeanalysis 29b

CAMAGBIBLIOGRAPHYSERVICE No.10416

104058 T.TOSTI,G.RAKIC,M.NATIC,D.MILOJKOVIC-OPSENICA,S.HUSINEC,V.SAVIC,Z.TESIC*(*FacultyofChemistry,UniversityofBelgrade,P.O.Box51,11158Belgrade,Serbia;ztesic@chem.bg.ac.rs):TLCretentionbehaviorofbrodifacoum,bromadiolone,andcoumatetra-lylandtheirimpuritiesondifferentadsorbents.J.PlanarChromatogr.22,���-�4�(2009).TLCofbrodifacoum,bromadiolone,coumateralylandimpuritiesonsilicagel,alumina,cellulose,andRP-18with46differentmobilephasesinatwintroughchambersaturatedfor�0min.Themostselectivephasesonsilicagelwerechloroform-ethylacetate-n-hexaneinvariousratios,ethylmethylketone-toluene1:9,andchloroform-toluene7:�;onaluminathebestmobilephasewasdichloromethane-n-hexane�:2.DetectionunderUVlightat254nm.

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104059 T.TUZIMSKI(DepartmentofPhysicalChemistry,FacultyofPharmacy,MedicalUniversityofLublin, 4 Staszica Street, 20-081 Lublin, Poland, tomasz.tuzimski@umlub.pl):Application ofSPE-HPLC-DAD and SPE-HPTLC-DAD to the analysis of pesticides in lake water. J. PlanarChromatogr.22,2�5-240(2009).HPTLCofpesticides(clofentezine,neburon,chlorfenvinphos,lenacyl,trifluralin,thiram,procymidone,flufenoxuron,tralkoxydim,propaquizafop,dinoseb)andwatersamples(samplepreparationbysolidphaseextraction)onsilicagelwithethylacetate-n-heptane1:4and�:7inahorizontalchamber.Quantitativedeterminationbydiodearrayden-sitometryintherangeof200to600nm.Thelimitofdetectionwasbetween40and650ng/spotandthelimitofquantificationwasbetween120and1920ng/spot.

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30. Syntheticandnaturaldyes104060 GertrudMORLOCK*,C.OELLIG(*UniversityofHohenheim,Garbenstrasse28,70599Stuttg-

art,Germany;gmorlock@uni-hohenheim.de):Rapidplanarchromatographicanalysisof25wa-ter-solubledyesusedas foodadditives. J.AOACInt.92,745-756 (2009).HPTLCof25dyes(brilliantblackBN,tartrazine,ponceau6R,resorcinyellow,fastyellowAB,orcein,allurared,greenS,amaranth,quinolineyellow,acidblue,erythrosine,sunsetyellowFCF,indigocarmine,ponceau4R,azorubine,brilliantblueFCF,carmine,scarletGN,copperchlorophyll,enocyanine,chlorophyllintrisodiumcoppersalt,curcumin,riboflavin-5-phosphate,riboflavin)onsilicagelinahorizontaldevelopingchamberwithethylacetate-methanol-water-aceticacid65:2�:11:1for40samplesin12min.Relativehumiditywas21+/-�%atatemperatureof20+/-�°C.Al-ternatively,atwintroughchamberorautomaticdevelopingchambercanbeused.Quantitativedeterminationbyabsorbancemeasurementat11differentwavelengths.Repeatabilities(%RSD,n=4)nearthelimitofquantificationshowedprecisionsofmostly0.9987) and RSD values (

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32. Pharmaceuticalandbiomedicalapplications104062 S.AGARWAL*,A.AIL,Y.DU,S.ABUJA(*Dept.ofPharmaceutics,FacultyofPharmacy,Ja-

mieHamdardUniversity,NewDelhi110062,India,agarwal_sp@yahoo.com):DeterminationofartemisinininbulkandpharmaceuticaldosageformsusingHPTLC.Ind.J.Pharma.Sci.71(1),98-100 (2009).HPTLCofartemisininonsilicagelwith toluene -ethylacetatewithchambersaturationfor�0min.Quantitativedeterminationbyabsorbancemeasurementat520nm.Theme-thodwaslinearovertherangeof100-600ng/band,recoverywasintherangeof98.8-100.5%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

10406� S.AHMAD*,M.SINGH,M.KAUR,A.AHMED(*JamiaHamdard,FacultyofPharmacy,NewDelhi,India):QuantitativeestimationofglycyrrhizicacidinthetabletsofYashtimadhubyHPT-LC.60thIndianPharmaceuticalCongressPG-260(2008).HPTLCofglycyrrhizicacidonsilicagelwithchloroform-glacialaceticacid-methanol-water15:8:�:2.Quantitativedeterminationbyabsorbancemeasurementat254nm.ThehRFvalueofglycyrrhizicacidwas28.Themethodwas linear in the rangeof50-500ng/spot.Thesampleanalyzedby theproposedmethodcon-tained87.8µgglycyrrhizicacidpertablet,equivalentto0.015%w/wofthetabletformulation.

qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2e

104064 S. AHMAD*, A. KAMAL, R. PARVEEN, F. AHMAD, K. SALEEM (*JMI, Dept. of Bio-sciences,NewDelhi,India):DevelopmentandvalidationofnovelHPTLCmethodforquantitativeestimationofstrychnineandbrucineinseedsofStrychnosNuxVomica.60thIndianPharmaceuti-calcongressPA-2�5(2008).HPTLCofstrychnineandbrucine(inseedsofStrychnosNuxVomica)onsilicagelwithchloroform-methanol-ammonia�8:2:1.Quantitativedeterminationbyabsor-bancemeasurementat258nm(strychnine,hRFvalue29)and271nm(brucine,hRFvalue21).Themethodwaslinearintherangeof100-1000ng/spot(bothcompounds).Themethodwassuitableforstandardizationofseveralherbalformulationscontainingnuxvomicaasaningredient.

herbal,HPTLC,densitometry,quantitativeanalysis �2e

104065 S.AHMAD*, M. SINGH, R. PARVEEN,Y. KAMAL (*Jamia Hamdard, Faculty of Pharma-cy, New Delhi, India): Quantitative estimation of withaferin a in the tablets ofAshwagandhabyHPTLC.60th IndianPharmaceuticalCongressPG-262 (2008).HPTLCofwithaferinA inAshwagandhaonsilicagelaluminumlayerwithtoluene-ethylacetate-formicacid5:5:1.Quan-titativedeterminationbyabsorbancemeasurementat214nm.ThechromatogramsofthetabletformulationshowedazonecorrespondingtostandardwithaferinA(hRFvalue�7)indicatingthepresenceofthesameintheherbalformulation.Linearitywasintherange50to500ng/spot.TheconcentrationofwithaferinAwas8.07µg/tabletand0.001�4%w/winthetabletformulation.

qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2e

104066 M.ALAVALA(KLEUniversity‘sCollegeofPharmacy,Belgaum,Karnataka,India):Newsta-bilityindicatinghigh-performanceliquidchromatographyandhigh-performancethin-layerchro-matographymethod for theestimationofolopatadinehydrochloride.AbstractNo.F-�09,61stIPC(2009).HPTLCofolopatadineHClonsilicagelwithmethanol-chloroform-25%ammo-nia80:20:1.ThehRFvaluewas46.Quantitativedeterminationbyabsorbancemeasurementat�01nm.Themethodwaslinearintherangeof100-900ng/band.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104067 B.ARUN*,A.SUGANTHI,A.FATHIMUNNISA,T.RAVI(*CollegeofPharmacy,SriRama-krishnaInstituteofParamedicalScience,Coimbatore,TamilNadu,India):Developmentofvali-datedHPTLCmethodfortheestimationofbuclizinehydrochlorideintabletdosageform.Abs-tractNo.F-276,61stIPC(2009).HPTLCofbuclizinehydrochlorideonsilicagelwithmethanol-chloroform-ammonia8:1:1%.Quantitativedeterminationbyabsorbancemeasurementat2�4nm.

CAMAGBIBLIOGRAPHYSERVICE No.10418

Thecalibrationcurvewaslinearintherangeof100-700ng/spot.Thelimitofdetectionandlimitofquantificationwere20and100ng/spot,respectively.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104068 J.BAGYALAKSHMI*,S.VIJAYARAJ,SajnaJOHN,T.RAVI(*SriRamkrishnaInstiuteofPara-medicalScience,CollegeofPhamracy,Coimbatore,Tamilnadu,India):Developmentandvalida-tionofsimultaneousestimationofparacetamol,aceclofenacandrabeprazoleincombinedtabletdosage formulationbyHPTLCmethod.60th IndianPhamraceuticalCongressPA-222 (2008).HPTLCofparacetamol,aceclofenacandrabeprazoleonsilicagelwithethylacetate-methanol-glacialaceticacid90:10:1.Quantitativedeterminationbyabsorbancemeasurementat275nm.Linearitywasintherangeof100-500µg/mL,20-100µg/mLand2-10µg/mLforparacetamol,aceclofenacandrabeprazolerespectively.Recoverywasintherangeof98.9-100.1%forallthreecompounds.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104069 N.BAIRWA*,A.TRIVEDI,S.MISHRA(*TheM.S.UniversityofBaroda,PharmacyDept.,Va-dodara,Gujarat,India):Simultaneousestimationofmarkersinahaematinicherbomineralformu-lationusinghigh-performancethin-layerchromatography.60thIndianPharmaceuticalCongressPG-251(2008).HPTLCofglycyrrhetinicacidandpiperineinhaematinicherbomineralcapsuleformulationonsilicagelwithtoluene-ethylacetate-glacialaceticacid25:15:1.QuantitativedeterminationbyabsorbancemeasurementatUV254nm.Themethodwaslinearintherangeof0.8-2.4ng/spot(glycyrrhetinicacid)and10-50ng/spot(piperine).Recoverywas96.�-98.6%.traditionalmedicine

herbal,HPTLC,densitometry,quantitativeanalysis �2e

104070 V.BALI*,M.ALI,J.ALI(*JamiaHamdard,FacultyofPharmacy,NewDelhi,India):AnovelandrapidHPTLCmethodfortheanalysisofrosuvastatincalcium.60thIndianPharmaceuticalCongressPA-219(2008).HPTLCofrosuvastatincalciumonsilicagelwithtoluene-ethylace-tate-formicacid9:7:1.Quantitativedeterminationbyabsorbancemeasurementat254nm.ThehRFvaluewas�2.Themethodwaslinearintherangeof100-100ng/spot,recoverywas99.7%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104071 V.BHAVNANI*,V.DIWALE,P.DESHMUKH,A.DHIWARE(*A.I.S.S.M.S.CollegeofPhar-macy, Pune, Maharashtra, India):Validated method development for estimation of famotidineanddomperidoneincombinedtabletdosageform.AbstractNo.F-��5,61stIPC(2009).HPTLCoffamotidineanddomperidoneonsilicagelwithtoluene-methanol-triethylamine12:6:1.ThehRFvaluewas2�and67forfamotidineanddomperidone,respectively.Quantitativedetermina-tionbyabsorbancemeasurementat290nm.Themethodwaslinearintherangeof100-500ng/band.Recoverywas98.6-98.9%forbothdrugs.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104072 D.BHAWSAR*,P.RATHI,M.PURANIK,P.YEOLE(*InstituteofPharmaceuticalEducationandResearch,Wardha,Maharashtra,India):DevelopmentandvalidationofHPTLCtechniqueforsimultaneousestimationofgatifloxacinandornidazoleinsoliddosageforms.AbstractNo.F-�47,61stIPC(2009).HPTLCofgatifloxacinandornidazoleonsilicagelwithdichloromethane-methanol-25%ammonia95:10:�.ThehRFvaluewas16and60forgatifloxacinandornidazole,respectively.Quantitativedeterminationbyabsorbancemeasurementat�02nm.Themethodwaslinearintherangeof20-200ng/bandforgatifloxacinand50-500ng/bandforornidazole.Reco-verywasbetween100.4and101.9forbothdrugs.

pharmaceuticalresearch,qualitycontrol,densitometry,HPTLC,quantitativeanalysis �2a

10407� R.BIDAWAI*,N.RAUT,D.WANKHEDE,N.GAIKWAD(*UniversityDept.ofPharmaceuti-calScience,RTMNagpurUniversity,Nagpur,Maharashtra,India):Validatedstabilityindicating

CAMAGBIBLIOGRAPHYSERVICE No.10419

HPTLCmethodfortheestimationofolmesartanmedoxomilinbulkandpharmaceuticaldosageform.60thIndianPharmaceuticalCongressPA-226(2008).HPTLCofolmesartanmedoxomil(anangiotensin-IIantagonist)onsilicagelwithtoluene-acetonitrile-methanol-ethylacetate-aceticacid(mobilephaserationotspecifiedbytheauthors).ThehRFvaluewas56.Quantitativedeterminationbyabsorbancemeasurementat262nm.The linearitywasbetween�00-800ng/spot.Themethodwassuitable forseparationofolmesartanmedoxomil fromdegradationpro-ductsobtainedbyforcedstressconditions(acid,alkali,peroxide,light,heat).

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104074 A.CHABUKSWAR*,S.JAGDALE,S.KUMBHAR,R.WAVHALE(*BombayCollegeofPhar-macy,Mumbai,Maharashtra,India):SimultaneousHPTLCestimationofcertainantihypertensivedrugs in tabletdosage form.60th IndianPharmaceuticalCongressPA-2�0 (2008).HPTLCofamlodipinebesylate(AB)andtelmisartan(TMS)onsilicagelwithethylacetate-1,4-dioxane-methanol-25%ammonia�0:�:6:�.ThehRFvaluewas16forTMSand��forAB.Quantitativedeterminationbyabsorbancemeasurement at �2�nm.Themethodwas linear in the rangeof100-500µg/mL(TMS)and200-1000µg/mL(AB),averagerecoverywas100.2-100.4%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104075 MrinaliniDAMLE*,K.BOTHARA,KirtiTOPAGI(*Dept. foChem.A.I.S.S.M.S.CollegeofPharma,KennedyRoad,R.T.O.Pune411044,India.,mcdamle@rediffmail.com):Stability-indi-catingHPTLCmethodfordeterminationofnebivololhydrochlorideandvalsartan.Ind.J.Phar-ma. Sci. 8(4), 198-201(2009). HPTLC of nebivolol hydrochloride and valsartan on silica gelwithethylacetate-methanol-aceticacid12:2:1inatwintroughchambersaturatedfor15min.Quantitativedeterminationbyabsorbancemeasurementat240nmforvalsartanand280nmfornebivololhydrochloride.Themethodwasfoundtobelinearintherangeof600-1400ng/bandfor valsartan 1200-2800 ng/band for nebivolol.The sample were subjected to different stressconditions (acid,alkali,oxidation,photolysis, thermal)andalldegradationproductswerewellseparatedfromthemaincompounds.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104076 R.S.DAREKAR,A.B.KHETRE,S.M.SINGH,M.C.DAMLE*(*DepartmentofPharmaceu-ticalChemistry,AISSMSCollegeofPharmacy,NearR.T.O.,KennedyRoad,Pune411001,India,mcdamle@rediffmail.com):HPTLCquantitationof2-hydroxy-4-methoxybenzaldehydeinHemidesmusindicusR.Br.rootpowderandextract.J.PlanarChromatogr.22,45�-456(2009).HPTLCof2-hydroxy-4-methoxybenzaldehydeandbiologicalextractsonsilicagelwithtoluene-ethylacetate-aceticacid7:2:1inatwintroughchambersaturatedfor20min.Quantitativedeter-minationbyabsorbancemeasurementat277nm.

herbal,traditionalmedicine,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2e

104077 P. DESHPANDE*, G. SHRIDHARAN, L.ANANDI, D. JADHAV, M. DAMLE, S. GANDHI(*Dept.ofPharmaceuticalAnalysis,AISSMSCollegeofPharmacy,KennedyRoad,Pune, In-dia,santoshvgandhi@rediffmail.com):Validatedmethoddevelopmentforestimationofatorvas-tatincalciumandfenofibrateinfixeddosecombinationbyHPTLC.ThePharmaReview7(�9),151-15�(2009).HPTLCofatorvastatincalciumandfenofibrateonsilicagel(pre-washedwithmethanol)withchloroform-methanol4:1over20mmwithchambersaturation.ThehRFvalueofatorvastatincalciumwas29andoffenofibrate77.Themethodwaslinearintherangeof200-1000ng/bandforatorvastatincalciumand�20-1600ng/bandforfenofibrate.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104078 S.R.DHANESHWAR*,V.K.BUSARI,M.V.MAHADIK(*BharatiVidyapeethUniversity,Poo-na College of Pharmacy, Department of Pharmaceutical Chemistry, Pune, Maharashtra, India4110�8; sunil.dhaneshwar@gmail.com): Application of a stability-indicating thin-layer chro-matographicmethod to thedeterminationof tenatoprazole inpharmaceuticaldosage forms. J.

CAMAGBIBLIOGRAPHYSERVICE No.10420

AOACInt.92,�87-�9�(2009).TLCoftenatoprazole-beforeandafteracidandalkalihydroly-sis,oxidationandphotodegradation-onsilicagel,prewashedwithmethanolanddriedat110°Cfor5min,withtoluene-ethylacetate-methanol6:4:1inatwintroughchambersaturatedwiththemob