2043 5 2 - moodle usp: e-disciplinas
Post on 20-Dec-2021
4 Views
Preview:
TRANSCRIPT
usP 33
ENTIFICATION IP on-The Sample is pre~ared as follows.] [N ,nple: Transfer a po~Ion of the melted Suppositories obS~ined in the Assay, equ1valent to 1 g of aspirin, to a 125-ml
nicai flask. Add 20 ml of_ alco~ol, and warm until comcfetely disinteg~ted. Cool 1n an ice bat~ for 5 min, filter, and ~vaparate the f1ltrat~ to dryness: the res1due meets the requirernents of the follow1ng tests.
• A. Heat the residue wi~h wate_r for several min, cool, and add 1 or 2 drops of teme chlonde TS: a violet-red color is produced.
• 8. INFIARED ABSORPTION (197K)
ASSAY • paOCEDURE
(NOTE-ln this Assay, use chloroform that recently was saturated with water.]
Chromatographic column: Uniformly pack a chromatographic tube, as described in the test for Procedure: Limit of Free Salicylic Acid, with a mixture of 3 g of chromatographic siliceous earth and 2 ml of sodium bicarbonate solution (1 in 12) prepared on the day of use.
Standard stock solution: Transfer 50 mg of USP Aspirin RS to a 50-ml volumetric flask, add 0.5 ml of glacial acetic acid, and add chloroform to volume.
Standard solution: O.OS mg/ml USP Aspirin RS from Standard stock solution diluted with a solution of glacial acetic acid in chloroform (1 in 100)
sample solution: Tare a small dish and glass rod, place in the dish NLT 5 Suppositories, heat gently on a steam bath until melted, then stir, and cool while stirring. Transfer a portion of the mass, equivalent to 50 mg of aspirin, to a 50-ml volumetric flask containing 1 ml of a solution of hydrochloric acid in methanol (1 in 50), add 40 ml of chloroform, and add chloroform to volume.
Spectrometric conditions (See Spectrophotometry and Light-Scattering (851 ).) Mode: UV Analytical wavelength: 280 nm Cell: 1 cm Blank: Chloroform
Analysis: Pipet 5 ml of the Sample solut!on i~to the column, wash with 5 ml of chloroform, then aga1n w1th 25 ml of chloroform, and discard the washings. Without delay, elute into a 100-ml volumetric flask with 1 O ml of a solution of glacial acetic acid in chloroform (1 in 1 O), and then with 85 ml of a solution of glacial acetic acid in chloroform (1 In 100), and dilute with the latter solvent to volume. Without delay, determine the absorbances of the eluted Sample solution and Standard solution. Calculate the percentage of (9HsO◄ in the portion of Suppositories taken:
Result = (Au/As) x (Cs/Cu) X 100
~ = absorbance of the Sample solution As = absorbance of the Standard solution Cs = concentration of USP Aspirin RS in the Standard
solution (µg/ml) . . . Cu = nominal concentration of aspmn 1n the Sample
solution (µg/mL) Acceptance criteria: 90.0<¾r 1 l 0.0%
IMPURITIES Organk lmpurftles ' PllocEDURE: LIMIT OF FREE SALICYLIC ACID
Ferric chloride-urea reagent: To a mixture of 8 ml of ferric chloride solution (6 in 10) and 42 ml of 0.05 N hydrochloric acid, add 60 g of urea. Dissolve t~e urea by ~irling and without the aid of heat,. ~nd ad1ust the resultmg solution, if necessary, by the add1t1on of 6 N hydrochloric acid to a pH of 3.2. [NOTE-Prepare on the day of use.]
Chromatographic column: lnsert a small pledget of glass wool above the stem constriction of a 20- x 2.5-cm chromatographic tube, and uniformly pack with a mixture of 1
Official Monographs / Aspirin 2043
. . . h and Q.5 ml of 5 M g of chromatograph1c s1hceous ea;. layer pack a similar phosphoric acid. Directly above ht. '
5silicedus earth, and 2
mixture of 3 g of chromatograp ,e ml of Fe"ic chloride~rea rea9enr suitable quantity of
Standard stock solutron: Dissobve_ ª a solution containing salicylic acid in chloroforrn to O tain 150 µg/ml of salicylic acid. f h Standard stock so/u-
Standard solution: Pipet 5 rnl O t e . . 10 rnl of tion into a 50-rnl volurnetric fla~k co~tami~gl O rnl of a methanol, 0.1 ml of hydr~h!orrc ac, ' ª!1
10 Add chlo-solution of glacial acetic ac1d m ether (1 in ). roform to volume. d I d lace in
Sample solution: Tare a small dish an 9 ass ro , P the dish NLT 5 Suppositories, heat ~ently ?n a steam rb!th
until melted, then stir, and cool wh1le st1rnng. T~a.nsfe ee portion of the mass equivalent to 50 mg of asp1nn (s Sample solution in the Assay) to a small beaker. Add 1 O ml
' · ·1 ct· 1 ed With of chloroform, warm slightly, and stIr untI isso v · the aid of 5 ml of chloroform, transfer to the chromat?· graphic adsorption column. Pass 50 m~ of chlor?form m several portions through the column, nnse the_ t1p of the chromatographic tube with chloroform, and d1scard the eluate. lf the purple zone reaches the botto~ of the tube, discard the column, and repeat the test w1th a smaller quantity of melted Suppositories. . Elute the adsorbed salicylic acid into a 100-ml volumetnc flask containing 20 ml of methanol an~ 0.2 ml of h~drochloric acid by passing two 10-ml portIons of a _solut1on of glacial acetic acid in water-saturated ether (1 1n 1 O), and then 30 ml of chloroform, through the column, and dilute the eluate with chloroform to volume.
Spectrometric conditions (See Spectrophotometry and Light-Scattering (851 ).) Mode: UV Analytical wavelength: 306 nm Cell: 1 cm Blank: A solvent mixture of the sarne composition as the Standard solution
Analysis Samples: Standard so/ution and Sample so/ution Concomitantly determine the absorbances.
Acceptance criteria: The absorbance of the Sample solution is NMT 3.0% that of the Standard solution.
ADDITIONAL REQUIREMENTS • PACKAGING AND STORAGE: Preserve in well-closed containers,
in a cool place. • USP REFERENCE STANDARDS (11)
USP Aspirin RS
Asplrln Tablets
DEFINITION Aspirin Tablets contain NLT 90.0% and NMT 110.0% of the
labeled amount of aspirin (C9HsO◄). Tablets of larger than 81-mg size contain no sweeteners or other flavors. [NOTE-Tablets that are enteric-coated meet the requirements for Aspirin Delayed-Release Tablets.]
IDENTIFICATION • A. PRocEDURE
Sample: 1 Tablet Analysis: Crush and boil Sample with 50 ml of water for 5 min, cool, and add 1 or 2 drops of ferric chloride TS.
Acceptance criteria: A violet-red colar is produced. • B. INFRARED ABSORPTION (197K)
Sample: Shake a quantity of finely powdered Tablets, equivalent to 500 mg of aspirin, with 1 O ml of alcohol for several min. Centrifuge_ the mixture. Pour off the clear supernatant, and evaporate It to dryness. Dry the residue in a vacuum at 60° for 1 h.
2044 Aspirin / Officia/ Monographs
ASSAY • PROCEDURE
Mobile phase: Dissolv 2 f d' in a mixture of 8S0 Le f 9 ° so ium 1-heptanesulfonate and adjust with glac~I O t"'."ate~dand 150 ml of acetonitrile, Diluent· A . . ace ,e ac, to a pH of 3.4.
St d . cetonitnle and formic acid (99·1) an ard solutlon· o 5 / · Sample stock solut· : ~g ~L of USP ~spirin RS in Diluent aspirin from finei ion. rans er an equ,valent to 100 mg of
contai~er. Add 2J cfº1dered_ Tablets (NLT 20), to a suitable orously for 10 . · md O Di(uent and 1 O beads. Shake vig-Sam 1 • mm, an centnfuge. tiori ;it~oiut1~n: Dilute .ª volume of the S~mple stock so/u-orr vo umes of Diluent. [NOTE-Relam the remaining PS
1. 'º,~ of Samp/e stock solution for the test for Limit of Free a 1cy IC Acid.]
Chromatographic system (See Chromatography (621 ), System Suitability) M~~ K · Detector: UV 280 nm Column: 4.0-mm x 30-cm; packing L 1 Flow rate: 2 ml/min lnjection size: 1 O µL
System suitablllty Sample: Standard solution Suitability requirements
Talling factor: NMT 2.0 Relative standard deviation: NMT 2.0%
Analysis Samples: Standard solution and Sample solution Calculate the percentage of ( 9HaO4 in the portion of Tablets taken:
Result = (ru/rs) x (Cs/Cu) x 100
ru = peak response of the aspirin from the Sample solution
rs = peak response of the aspirin from the Standard solution
Cs = concentration of USP Aspirin RS in the Standard solution (mg/ml)
Cu = nominal concentration of the Sample solution (mg/ml)
Acceptance criteria: 90.0%-110.0%
PERFORMANCE TESTS • DISSOLUTION (711)
O.OS M acetate buffer: Mix 2.99 g of sodium acetate trihydrate and 1.66 ml of glacial acetic acid with water to obtain 1000 ml of solution having a pH of 4.50 ± O.OS.
Medium: 0.05 M acetate buffer; 500 ml Apparatus 1 : 50 rpm Time: 30 min Standard solution: USP Aspirin RS of a known concentration in Medium [NOTE- Prepare the Standard solution at the time of use. An amount of alcohol not to exceed 1 % of the total volume of the Standard solution may be used to bring the Reference Standard into solution before dilution with Medium.] . • h sample solution: Sample per Dissolution (711 ). D1lute w1t Medium, if necessary, and f1lter.
Analysis . Samples: Standard solution and Sa~ple solut,on Determine the amount of ( 9HaO4 d1s~olved f~om ~V absorbances at the wavelength of the 1sosbest1c pomt of aspirin and salicylic acid at 265 ± 2 nm of th~ Sample solution in comparison with the Standard solut,on.
Tolerances: NLT 80% (Q) of the labeled amount of ( 9Hs0 4 is dissolved.
• UNIFORMITY OF DOSAGE UNJTS (905): Meet the requirements
IMPURITIES Organlc lmpurltles • PROCEDURE! LIMIT OF fRH SAUCYLIC ACID . . Mobile phase and Diluent: Prepare as directed ,n the
Assay.
Usp 33
Standard solution: 0.015 mg/!'f1L of s~licylic acid in the Standard solution prepared as directed m the _Assay.
Sample solutlon: Use the Sample stock solut,on from the Assay. d d' Chromatographlc system: Procee as irected in lhe Assay.
System sultablllty . Sample: Standard solut,o~ . . . [Non-The relative retentIon times for_sahcyhc acid and aspirin are about 0.7 and 1.0, respect1vely.]
Sultablllty requirements . . . Resolutlon: NLT 2.0, between sallcyhc :c1d and aspirin Relatlve standard deviatlon: NMT 4.0 ¾> for the salj. cylic acid peak responses
Analysls Samples: Standard solution and Sa,:nple soluti~n Calculate the percentage of C1H6O3 m the portIon of Tab. lets taken:
Result = (ru/rs) x (Cs/Cu) x 100
ru = peak response of the salicylic acid from the Sample solution
rs = peak response of the salicylic acid from the Standard solution
Cs = concentration of USP Salicylic Acid RS in the Standard solution (mg/ml)
Cu = concentration of aspirin in the Sample solution as determined in the Assay (mg/ml)
Acceptance criterla: NMT 0.3%. For Tablets that are coated, NMT 3.0%.
ADDITIONAL REQUIREMENTS • PACKAGING AND STORAGE! Preserve in tight containers. Pre
serve flavored or sweetened Tablets of 81-mg size or smaller in containers holding NMT 36 Tablets each.
• USP REFERENCE STANDARDS (11) USP Aspirin RS USP Salicylic Acid RS
Buffered Asplrln Tablets DEFINITION Buffered Aspirin Tablets contain Aspirin and suitable buffering
agents. Tablets contain NLT 90.0% and NMT 11 O.O% oi the labeled amount of aspirin (C9H8O4).
IDENTIFICATION • A. PROCEDURE
Sample: 1 Tablet An~lysis: Crush and boil Sample with 50 ml of water for 5 mm, coo!, and add 1 or 2 drops of ferric chloride TS.
Acceptance criterla: A violet-red color is produced. • B. INFRARED ABSORPTION (197K)
Sam1;>le: Shake a quantity of finely powdered Tablets, equ1valent to_ 500 mg of aspirin, with 1 o ml of Chloroforrn for severa! mm. Centrifuge the mixture. Pour off the clear supernatant, and evaporate it to dryness. Dry the residue in a vacuum at 60° for 1 h.
ASSAY • PROCEDURE
~obile _phase: Dissolve 2 g of sodium 1-heptanesulfonate m ª m,~ture ?f 850 ml of water and 150 ml of acetonitrile, ªnd adiust w,th glacial acetic acid to a pH of 3.4.
Dlluent: Acet?nitrile and formic acid (99: 1) Standard solut1on: 0.5 mg/ml of USP Aspirin RS in Oiluent Samp)e stock solution: Transfer an equivalent to 100 rng 01 aspin~, from finely powdered Tablets (NLT 20), to a suita~le contamer. Add 2~.0 ml of Di/uent and 10 beads. Shake vig· orously for 1 O mm, and centrifuge.
top related