biocommaIntroduction
Sulfonamides, cost-effective and widely used in pig farming,can accumulate in Beef, posing health risks. While SPEcartridges have been the conventional method for purifyingsulfonamide, the increasing use of QuEChERS in pesticideresidue analysis has prompted customers to seek itsapplication in veterinary drug residue analysis.Biocomma has developed a QuEChERS method to detect 19residues of sulfonamide veterinary drugs in Beef. The recoveryrate is 76-110% with RSD less than 10% for your reference.
Experiment
Extraction (Copure® QuEChERS, Cat. #: COQ050050H)
Weight 2.0 g of ground Beef into a 50 mL centrifuge tube.Added 4 mL of water, and vortex for 1 min. Add 10 mL of 1%acetic acid acetonitrile, and vortex for 1 min. Add QuEChERSextraction salt. Vortex to mix well. Extract by ultrasonictreatment for 10 min, and centrifuged at 5000 r/min for 2 min.The sample is ready for purification.
Purification (Copure® QuEChERS, Cat. #: COQ015427H)
Add 5 mL of prepared supernatant and the QuEChERSpurification salt into a clean tube. Vortex at 2500 r/min for 2min, then centrifuge at 8000 r/min for 5 min. Evaporate 2 mLof supernatant to nearly dryness. Dilute to 1 mL by methanolsolution with 0.1% formic acid (water: methanol = 9:1). Thesample is ready for analysis.
Preparation of Standard Curve Solution
Prepare blank sample in the same procedures. Add internalstandard to prepare the concentrations of 2 μg/L, 5 μg/L, 10μg/L, 20 μg/L, 50 μg/L and 100 μg/L.
Instrumental Conditions
1.Chromatographic conditions
Instrument: UPLC-MS/MS (Thermo Fisher TSQ Endura)
Chromatographic column: SinoPak BEH T-C18 (2.1 mm×100mm, 3 μm)
Mobile phase A: water containing 0.1 % formic acid
Mobile phase B: methanol-acetonitrile solution containing 0.1%formic acid (methanol: acetonitrile=2:8)
Flow rate: 0.3 mL/min
Column temperature: 35 ℃
Injection volume: 10 μL
Table 1. Gradient Elution Program
1.Mass Spectrometry Conditions
Ion source: HESI
Electrospray voltage: 3500 V
Sheath gas pressure: 40 arb
Auxiliary gas pressure: 2 arb
Ion exchange tube: 380 ℃
Auxiliary air temperature: 350 ℃
Table 2. Targets, Retention Times and Characteristic Ions (* isQuantitative Ions)
Results
Table 3. Spiked Recovery of 19 Residues of Sulfonamide in Beef
Ordering Information
