biocommaIntroduction
Sulfonamides, cost-effective and widely used in pig farming,can accumulate in Beef, posing health risks. High fat andphospholipid in Beef complicate residue detection. Theaccumulated phospholipid on chromatographic column notonly reduces lifespan, but also causes ion suppression in massspectrometry, resulting in low recovery rates and impacting thesensitivity and reproducibility of instrumental analysis.
Biocomma has developed a QuEChERS method withsimplified operation and good recovery to effectively removephospholipids, adsorb lipids, and detect 19 residues ofsulfonamide veterinary drugs in Beef. The spiked recoveries atboth 5 ng/g and 10 ng/g were 60-120 % 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 2 min. Add 10 mL of 1%acetic acid acetonitrile, and vortex for 10 min. Add QuEChERSextraction salt. Vortex for 2 min, and centrifuged at 5000 r/minand 4 ℃ for 5 min. Let stand for 15 minutes, then the upperacetonitrile layer is ready for purification.
Purification (Copure® QuEChERS, Cat. #: COQ015427H)
Add 6 mL of prepared supernatant and the QuEChERSpurification salt into a clean tube. Vortex for 2 min, thencentrifuge at 5000 r/min for 5 min. Evaporate 4 mL ofsupernatant to nearly dryness at 40 ℃ . Dilute to 1 mL bymethanol solution with 0.1% formic acid (water: methanol =9:1). Filter by a 0.22 μm membrane. The sample is ready foranalysis.
Instrumental Conditions
1.Chromatographic Conditions
Instrument：UPLC-MS/MS (Thermo Fisher TSQ Endura)Chromatographic column：Commasil® veterinary drug residuesspecial columns (2.1 mm×100 mm, 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 °C
Injection volume: 10 μL
Table 1. Gradient Elution Program
2.Mass Spectrometry Conditions
Ion source：HESI
Electrospray voltage：3500 V
Sheath gas pressure：40 arb
Auxiliary air pressure：2 arb
Ion exchange tube：380 ℃
Auxiliary air temperature：350 ℃
Table 2. Targets, Retention Times and Characteristic Ions (* isthe Quantitative Ion)
Table 3. Results of Spiked Recovery of 19 Residues of Sulfonamide Veterinary Drugs
Ordering Information
