Introduction

Comparing to traditional SPE cartridges, Copure® HLB LimCartridges for Multi-Residue Analysis of Veterinary Drugremove various interferers such as fats, phospholipids,and pigments more rapidly to reduce the matrix effect. Thepreparation procedures have been simplified to save cost andtime by skipping activation and equilibration.

Through low, medium, and high level spiked experiments,the target compounds of 36 veterinary drug residues such astetracyclines, sulfonamides and quinolones in Beef and shrimphave been determined. Biocomma established a UPLC-MS/MSmethod with good recovery and precision for your reference.

Experiment

Extraction

Accurately weigh 1 g of the ground sample into aclean centrifuge tube. Add 5 mL of 0.2% formic acid inacetonitrile:water (80:20, v/v) and vortex to mix well. Then,extract by ultrasonic treatment for 20 min, and centrifuge at8000 r/min for 5 min. The sample is ready for purification.

Purification (Copure® HLB Lim, 200 mg/ 3 mL)

Pipette 2.5 ml supernatant of extracted sample to aCopure®HLB Lim Cartridge. Collect the filtrate and evaporateto dryness. Redissolve to 1 mL by 0.1% formic acid in watermethanol (9:1). After filter by membrane, the sample is readyfor UPLC-MS/MS analysis.

Preparation of Standard Curve Solution

Prepare blank sample in the same procedures. After collectingthe eluent, add internal standard solution. Evaporate and dilutethe concentration of 2 μg/L, 10 μg/L, 50 μg/L, 100μ g/L, 200 μg/L, and 500 μg/L.

Instrument Conditions

1.Chromatographic Conditions

Instrument: UPLC-MS/MS (Thermo Fisher TSQ Endura)

HPLC column: Commasil® Specialized Column for VeterinaryDrug Residues (2.1 mm×100 mm, 3μm)

Mobile phase A: water (0.1% formic acid)

Mobile phase B: 0.1% formic acid solution in methanolacetonitrile (2:8)

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 transfer tube: 380 ℃

Auxiliary gas temperature: 350 ℃

Table 2. Targets, Retention Times and Characteristic Ions(*Quantifier Ion)

Results

Table 3. Spiked 36 Veterinary Drugs Resides Recover

Ordering Information

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