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Food and Beverage ApplicationsSulfonamide Antibiotic Residues in Milk on Acclaim 120 C18Antioxidants in Edible Oils by AOAC 983.15 on Acclaim 120 C184012 3 4 5C6 7 8mAUB*0A5 10 15 20 25MinutesColumn: Acclaim 120 C18, 5 µm,4.6 × 250 mmPump: Summit P580 HPG/4Mobile Phase: (A) 30 mM acetic acidadjusted to pH 4.2 with NaOH(B) MethanolGradient Times: 0.0 20 25%A 88 60 60%B 12 40 40Flow: 1.5 mL/minTemperature: 35 °CInjection: ASI-100 autosampler, 100 µLDetector: UVD 340U, UV at 265 nmwith spectral confirmationSample Prep.: AOAC 993.32; refer to procedurefor important notesSamples: (A) Spiked extract of skim milk,1.0 µg/g each(B) Milk extract(C) Sulfonamide standards,0.20 µg/mL in waterPeaks: 1. Sulfadiazine (SDZ)2. Sulfathiazole (STZ)3. Sulfapyridine (SPD)4. Sulfamerazine (SMR)5. Sulfamethazine (SMZ)6. Sulfachloropyridazine (SCP)7. Sulfadimethoxine (SDM)8. Sulfaquinoxzline (SQX)*. TheobromineNote: Most interferences are organic acids thatmay be moved out of the way by smalladjustements to the pH of the mobile phase.21533Background Information: Nine antioxidants forAOAC 983.15 spiked into wheat germ oil.Column: Acclaim 120 C18, 5 µmDimensions: 4.6 × 150 mmMobile Phase: (A) 0.75% HOAc in H 2 O(B) 50/50/0.5 MeOH/acetonitrile/HOAcInj. Volume: 10 µLDetection: UV, 280 nm; diode array confirmationGradient:Time % A % B Flow0.0 30 70 2.09.6 0 100 2.011.4 0 100 2.012.0 0 100 4.017.0 0 100 4.01502713 456mAU01 232.5 Minutes4567Peaks: 1. Propyl gallate2. THBP3. TBHQ4. NDGA5. BHA6. Ionox-1007. Octyl gallate8. BHT9. Dodecyl gallate98Note: Ethoxyquin (not shown) has been resolved under the same conditions.89Extract of SpikedWheat Germ OilExtract ofWheat Germ OilStandards, 100 ng each1520404Bitter Principles in Beer on Acclaim 120 C18550 StandardsmAU ICS-H1ICS-R1ICS-T2ICS-I206.5 Märzen-style beer1 2mAU300 10 20 30MinutesColumn: Acclaim 120 C18 5µm,4.6 × 150 mmPump: Summit P680A DGP-6Mobile Phase: 75% methanol, 24% water,1% phosphoric acid (v/v/v)Flow: 1.2 mL/minTemperature: TCC-100 thermostat, 35 °CInjection: ASI100 autosampler, 25 µLDetector: UVD-340U, UV 270 nm;spectra 200–400 nmStandards*:ICS-I2: isohumulones 205 µg/mLICS-T2: tetrahydroisohumulones 135ICS-R1: rho-isohumulones 200ICS-H1: hexahydroisohumulones 210Peaks: 1. Isocohumulone2. Mixed isohumulone congeners3. IsoadhumuloneSample Preparation:Extraction per ASBC- 10 mL beer + 1 mL 3N HCl + 50 µL 1-octanol +20 mL iso-octane- Shake vigorously- Centrifuge to separate phases- Bitterness Units = 50 × A 275For HPLC- Evaporate dry and reconstitute in mobile phase*Obtained from Am. Soc. Brewing Chemists22027APPLICATIONSwww.dionex.com - 41 -