biocommaIntroduction
Sulfonamide, quinolone and tetracycline antibiotics arecommon human-animal antibiotics, used in both humansand animals. Due to their cost-effectiveness and effectiveantimicrobial properties, they are widely employed inaquaculture. Biocomma optimized the QuEChERS method withrecovery rate of 60%~110% and RSD less than 10% for yourreference.
Experiment
Extraction (Copure® QuEChERS, Cat. #: COQ050051H)
Weigh 2.0 g of pulverized meat sample in a 50 mL centrifugetube. Add 2 mL of Na2EDTA-Mcllvaine buffer (pH=4), thenvortex for 1 min. Add 10 mL of 1% acetonitrile acetate solution.Vortex for 1 min, then add the QuEChERS extraction salt.Vortex to mix well. Extract by ultrasonic treatment for 10 min,and centrifuge at 5000 r/min for 2 min. The sample is ready forpurification.
Purification (Copure® QuEChERS, Cat. #: COQ015605H)
Add 6 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 5 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 Matrix Standard Curve Solutions
Prepare blank sample in the same procedures. Add internalstandard to prepare the concentrations of 2 μg/L, 10 μg/L, 50μg/L, 100 μg/L, 200 μg/L, and 500 μg/L for standard curve.
Instrumental Conditions
1.Chromatographic Conditions
Instrument: UPLC-MS/MS (Thermo Fisher TSQ Endura)
Chromatographic column: Commasil® Veterinary ResiduesColumn BEH T-C18 (2.1 mm×100 mm, 3 μm)
Mobile phase A: water (containing 0.1 % formic acid)
Mobile phase B: methanol: acetonitrile = 2:8 (containing 0.1 %formic acid)
Flow rate: 0.3 mL/min
Column temperature:35℃
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 gas pressure: 2 arb
Ion exchange tube: 380 ℃
Auxiliary air temperature: 350 ℃
Table 2. Targets, Retention Times and Characteristic Ions(Quantitative Ion)
Results
Table 3. Results of Spiked Recovery of Multi- Residues of Veterinary Drug
Ordering Information
