高效液相色谱-串联飞行时间质谱高通量筛查生鲜乳中兽药残留

建立了一种高通量检测生鲜乳中兽药残留的高效液相色谱-串联飞行时间质谱方法，包括17大类兽药，共174?种。样品用乙腈和乙酸乙酯提取，冷冻净化后，目标化合物经过Poroshell 120 EC-C18柱（3.0?mm×150?mm，2.7?μm）分离，经0.1%甲酸溶液和甲醇流动相洗脱，采用电喷雾正离子模式进行采集。结果显示，114?种兽药化合物在质量浓度0～200?ng/mL范围线性良好（R2＞0.990?0），检测限为1～10?ng/g。此外，回收率在70%～130%范围内的质控加标样品达99?种，相对标准偏差为1.03%～9.65%。该方法检测速度快、灵敏度高，大大提高了生鲜乳中兽药筛查的效率。

High-Throughput Screening of Veterinary Drug Residues in Raw Milk by HPLC-TOF-MS/MS

In this study, a high performance liquid chromatography tandem time-of-flight mass spectrometry (HPLC-TOF-MS/MS) method was established for the high-throughput determination of 174 veterinary drug residues in raw milk. The target compounds were extracted with acetonitrile and purified by freezing. A Poroshell 120 EC-C18 column (3.0 mm × 150 mm, 2.7 μm) was used for the separation of the target compounds with a mobile phase consisting of 0.1% formic acid in water and methanol via gradient elution. The analytes were detected with an electrospray ionization source (EIS) in the positive ion mode. The results showed that the method had a good linearity (R2 > 0.990 0) and low limits of detection (LOD) (1–10 ng/g) for 114 pesticide compounds. The average recoveries for 99 of these ranged from 70% to 130% with relative standard deviation (RSD) from 1.03% to 9.65% at quality control concentration levels. The method was successfully applied in the screening of veterinary drug residues in raw milk with high efficiency and sensitivity.