News On Food2013 Volume 1

Food & Beverage

Analytical testing is used in the production of worldwide food supply – from raw materials and ingredients, to finished and packaged goods. This testing primarily serves two purposes: to determine nutritional value and quality, and to guarantee safety. Sigma-Aldrich®, through its Supelco® and Fluka® brands, is very active in product development for food and beverage analysis.

Food Chemistry

Comprehensive Determination of Trans Fats in food using Silver-Ion SPE Fractionation, SP™-2560 and SLB®-IL111 GC ColumnsA procedure used to determine trans fat levels involves extraction, derivatization, fractionation, and GC analysis.

•Silverion (Ag-ion) fractionation is applied to the FAMEs to separate the saturates and C18 trans monoenes in fraction 1, the cis monoenes in fraction 2, and the dienes in fraction 3.

•GC analysis of each fraction is then performed on an ionic liquid column. This extremely polar GC capillary column was the world’s first commercial column to rate over 100 on our GC column polarity scale. As such, it has the most orthogonal selectivity compared to commonly used non-polar and intermediate polar columns, providing increased selectivity for polar and polarizable analytes. The 100 m version is a great complementary column to the SP-2560.

Chromatograms obtained from the preparation of a commercially purchased cookie sample are shown. Peaks were identified using retention time and direct comparison to standards.

To read more about analysis of fats, visit sigma-aldrich.com/food-fats

Figure 1. GC Analysis inj. temp.: 250 °C detector: FID, 250 °C carrier gas: hydrogen, 1 mL/min injection: 1 μL, 10:1 split liner: 4 mm I.D., split type,

single taper wool packed FocusLiner™ design

t4 t5

t6-8

t9t10

t11

t12

t13-14

t15t16

Fraction 1 = C18:1 trans isomers

17 18 19 20 21

Min

c4-5 c6-7

c9

c11

c10

c12

c13 c14 c15 c16

Fraction 2 = C18:1 cis isomers

SP-2560, 100 m x 0.25 mm I.D., 0.20 μm (24056) at 180 °C isothermal, the AOCS method-specified column and oven temperature

t4 t5

t7

t8-9

t10

t11

t12

t13-14

t15 t16

t6

Fraction 1 = C18:1 trans isomers

c4

c9

c11c10

c12

c13 c14c15 c16c5

c6-7

c8

14 15 16

Min

Fraction 2 = C18:1 cis isomers

SLB-IL111, 100 m x 0.25 mm I.D., 0.20 μm (29647-U) at 168 °C isothermal, the experimentally-determined optimal oven temperature

GC Column Polarity Scale Visual Representation

Non-Polar

Intermediate Polar Polar Highly Polar Extremely Polar

sigma-aldrich.com/il-gc

0 65 100 32 10

-Octyl 280°C

-5 360°C

-20 300°C

-1701 280°C

-35 300°C

-50 310°C

-225 240°C

PAG 220°C

PEG 280°C

-2330 250°C

-2331 275°C

TCEP 145°C

-2560 250°C

-1 350°C

SLB-IL59 300°C

SLB-IL76 270°C

SLB-IL82 270°C

SLB-IL100 230°C

SLB-IL111 270°C

SLB-IL61 290°C

GC Column Polarity Scale (Visual Representation)

sigma-aldrich.com/analytical

News on Food | Volume 1

Simple Sugars Using Hydrophilic Interaction Chromatography (HILIC)Chromatographic analysis of simple sugars can be challenging because these compounds are highly polar, uncharged, and lack a chromophore. The preferred mode of HPLC separation is HILIC because it provides the advantage of retaining these highly polar compounds that are otherwise hard to separate.

•Polymeric columns bonded with aminopropyl groups offer improved stability and MS compatibility. Our apHera NH2 column is based on covalently bonded polyamine to co-polymer which offers stability from pH 2-12, mechanical and chemical strength, and high column efficiency.

•For faster analysis on any HPLC system, turn to Ascentis® Express. These columns, based on Fused-Core® technology, offer the performance of sub-2 μm particles but exhibit the backpressure of 3 μm particles. Several phases (HILIC, OH5, and F5) are available that are suitable for operation in the HILIC mode.

•The Ascentis Express F5 phase is also available in a more traditional 5 μm particle. The Fused-Core technology results in increased efficiency, whereas the 5 μm particles exhibit limited backpressure, allowing longer column lengths than that possible with the standard 2.7 μm Ascentis Express particles. To learn more, visit sigma-aldrich.com/express.

To read more about analysis of simple sugars, visit sigma-aldrich.com/sugars

Water Determination in Milk and Milk Products

Karl Fischer Titration with HYDRANAL® Reagents

In the production of milk and dairy products, water content plays an important role, technologically as well as economically. Therefore, national and international laws and agreements protect and regulate the definition of products and the production processes in dairy technology. Determining the water content in milk and milk products can be easily achieved with Karl Fischer (KF) titration.

The HYDRANAL line of products is adapted to these analyses.

Benefits

•Effective on all types of food substances

•Rapid, accurate, and precise measurements

•Measures the complete water content, including chemically combined water, but not other volatile substances (an advantage over drying methods)

• Includes many auxiliary reagents for enhancing sample solubility and speed of the titration

Our HYDRANAL service lab in Germany provides customer support in the use of HYDRANAL reagents and KF techniques.

To request the following milk and dairy application reports, visit sigma-aldrich.com/hydranal

•L074 Quark (cheese)

•L077 Whey fat emulsion

•L081 Milk powder (whole milk)

•L082 Milk powder (skim milk)

•L085 Milk

•L095 Cheese

•L097 Yogurt

•L222 Coffee cream

•L493 Whey (powdered)

•L523 Ice cream

Figure 2. Analysis of the Energy Drink Rock Star Using Ascentis HILIC (Si) with UV and ELSD Detection in Series

column: Ascentis Express HILIC (Si), 10 cm x 3.0 mm I.D., 2.7 µm particles (53970-U) mobile phase: (A) 100 mM ammonium acetate, pH 5.0 with acetic acid; (B) water; (C) acetonitrile; (9:1:90, A:B:C) mixing proportions: A:B:C = 9:1:90 flow rate: 0.6 mL/min pressure: 815 psi temp.: 35 °C det.: UV at 254 nm; ELSD, 55 °C, 3.5 bar nitrogen injection: 2 µL sample: dilute 1:9 in acetonitrile

910

87

0 5 10Min

7. Fructose 8. Glucose 9. Sucrose 10. Taurine

ELSD Detection

G005566

0 2 4 6 8 10Min

3

4

2

1

6

5

UV 254 nm Detection

1. Caffeine 2. Niacinamide (vitamin B3) 3. Pyridoxine hydrochloride (vitamin B6) 4. Benzoic acid 5. Sorbic acid 6. Riboflavin (vitamin B2)

G005565

3

Food Safety

Supel™ QuE Z-Sep QuEChERS Tubes:

Fat Removal in Difficult Matrices

Key Features and Benefits

•Useful for pesticide residue analysis

•Proprietary technology, significantly diminishes interference from fatty matrices and pigments

•Employs “Quick Easy Cheap Effective Rugged Safe” QuEChERS methodology

Technology OverviewSupel QuE Z-Sep/C18 and Z-Sep+ enhance sample cleanup for complex matrices by effectively removing more fat and color from sample extracts than traditional phases for QuEChERS LC-MS methods. By eliminating problematic matrix interferences, Z-Sep products provide more robust LC-MS methods. This proprietary technology can replace C18 and PSA phases in your current methods without additional method development.

Supel QuE Z-Sep/C18, a combination of Discovery® DSC-18 and Z-Sep particles, is recommended for samples containing <15% fat. Supel QuE Z-Sep+, C18 and Z-Sep dual bonded to silica, is recommended for cleanup of samples containing >15% fat.

12 14 16 18 20 22 24Time (min)

PSA/C18 Cleanup

12 14 16 18 20 22 24

Time (min)

Z-Sep+ Cleanup

column: SLB-5ms, 20 m x 0.18 mm I.D., 0.36 µm (28576-U) oven: 70 °C (2 min), 15 °C/min to 325 °C (5 min) inj. temp.: Programmed, 60 °C (0.28 min), 600 °C/min to 325 °C (5 min) detector: MS (SIM mode) carrier gas: helium, 1 mL/min constant injection: 10 µL LVI, PTV solvent vent, rapid injection speed; split vent flow: 100 mL/min (5 psi) until 0.28 min, 60 mL/min at 2.78 min liner: 4 mm I.D., split type, wool packed FocusLiner™ with single taper design

Figure 3. GC-MS Chromatograms (same y-axis)

For more information, request application note OXN.

To learn more, visit sigma-aldrich.com/food-pesticides

Figure 4. Bisphenol A Standard at 1 μg/mL

column: Ascentis Express C18, 10 cm x 2.1 mm I.D., 2.7 µm (53823-U) mobile phase: water:acetonitrile (60:40) flow rate: 0.4 mL/min. pressure: 3268 psi (225 bar) column temp.: 35 °C detector: UV (230 nm); FL (Ex 225 nm, Em 310 nm) injection: 1 µL sample: bisphenol A at 1 µg/mL in acetonitrile

Figure 5. Drinking Water Spiked with 0.2 µg/mL Bisphenol A

sample/matrix: Drinking water spiked with bisphenol A to a 0.2 µg/mL level SPE Tube: Supelclean ENVI-18, 500 mg, 6 mL glass tube, PTFE frit

(54331-U) condition: 1 mL 1% formic acid in acetonitrile, 1 mL DI water sample addition: 5 mL spiked water sample elution: 2 mL 1% formic acid in acetonitrile eluate post-treatment: 1 mL evaporated, then reconstituted to 0.5 mL with

acetonitrile

0 1 2 3Min

1. Bisphenol A UV Trace FL Trace

1

1

0 1 2 3Min

UV Trace FL Trace

11

Bisphenol AA fast procedure for determining bisphenol A in drinking water employs materials and techniques selected in part for speed, but also those that do not contribute unwanted artifacts. The use of ENVI-18 SPE allows BPA to be extracted and concentrated, which results in greater method sensitivity compared to simple direct injection or headspace methods. Using the calibration factor generated for the FL detector, a recovery of 88% was calculated.

For more information, request our flyer code ORB.

©2013 Sigma-Aldrich Co. LLC. All rights reserved. SIGMA, SAFC, SIGMA-ALDRICH, ALDRICH, and SUPELCO are trademarks of Sigma-Aldrich Co. LLC, registered in the US and other countries. FLUKA, TraceSELECT, TraceSELECT ULTRA, PERDROGEN, CHROMASOLV, FIXANAL, HYDRANAL, Riedel-de Haën, IDRANAL, SPECTRANAL, and VOLPAC are trademarks of Honeywell Specialty Chemicals Seelze GmbH. Sigma brand products are sold through Sigma-Aldrich, Inc. SLB, Ascentis and Hydranal are registered trademarks of Sigma-Aldrich Co. LLC. SP and Supel are trademarks of Sigma-Aldrich Co. LLC. Fused-Core is a registered trademark of Advanced Materials Technology, Inc. Purchaser must determine the suitability of the product(s) for their particular use. Additional terms and conditions may apply. Please see product information on the Sigma-Aldrich website at www.sigmaaldrich.com and/or on the reverse side of the invoice or packing slip.

Order/Customer Service (800) 325-3010 • Fax (800) 325-5052 Technical Service (800) 325-5832 • sigma-aldrich.com/techservice Development/Custom Manufacturing Inquiries (800) 244-1173 Safety-related Information sigma-aldrich.com/safetycenter

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Mycotoxin

Mycotoxins are products by fungal genera like Aspergillus, Fusarium, Penicillium, etc. These toxic secondary metabolites are harmful to animal and human health if they enter the food chain via contaminated crops and fruits or through processed food and feed products. Therefore, many countries have set limits regarding the level of mycotoxins found in food and feed. For a precise detection of all regulated mycotoxins, Sigma-Aldrich offers a comprehensive range of standards, including mixture solutions, 13C-isotopically labeled standards, certified reference materials (CRM) and dried down standards.

Download your Mycotoxin Standards Guide at sigmaaldrich.com/mycotoxins

Mycotoxin Standards

Single and Multi-Component Standard Solutions

13C - Isotopically LabeledStandards

Matrix Certified Reference Materials

Dried Down Standards

Additional LiteratureNEW – Supel™ Tox SPE Cartridges

Often, mycotoxin samples are purified and concentrated using Immunoaffinity (IAC)columns, but an alternative to this type of sample preparation method has been developed. Request a copy of our Supel Tox SPE brochure to learn more.

Food and Beverage Analysis Brochure

Request your copy of our Food and Beverage Analysis brochure to learn about simplified solutions to sample preparation while increasing speed and sensitivity.

Request these pieces and more by visiting sigma-aldrich.com/lit-request

Fast and Simple Cleanup for Mycotoxin Analysis

Supel™ Tox SPE Cartridges

11644_Supel Tox Brochure.indd 1 2/25/2013 10:49:09 AM

Food and Beverage AnalysisIncrease speed and sensitivity with proven solutions

Food Chemistry

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Adulterants

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Food & Beverage