液相色谱-四极杆/飞行时间质谱快速筛查饲料中36种违禁药物

Rapid Screening of 36 Forbidden Drugs in Feeds by Using Liquid Chromatography-Quadrupole/Time-of-flight Mass Spectrometry

建立了饲料中β-受体激动剂、激素共36种违禁药物的液相色谱-四极杆/飞行时间质谱(LC-Q-TOF/MS)的快速筛查方法。均质饲料样品中加入乙腈和混合吸附剂,经涡旋分散、振荡提取、离心和浓缩步骤,实现了36种药物的同时提取和净化(改良的QuEChERS方法)。提取液以甲醇-0.1%甲酸为流动相进行梯度洗脱,C18色谱柱(150 mm×2.1 mm,2.7μm)分离,采用正离子模式检测分析。在100～1 000 Da质量范围内进行一级和二级质谱全扫描。以分子离子峰的精确质量数提取的色谱图峰面积定量,以二级质谱特征子离子和保留时间定性。36种药物的质量数误差绝对值小于7.3 ppm,在10.0～200.0μg/kg范围内线性关系良好,相关系数大于0.99。3个浓度水平的平均回收率为65%～120%,相对标准偏差不高于24%。该方法操作简便、结果准确,适用于饲料中违禁药物的高通量快速筛查分析。

A liquid chromatography-quadrupole/time-of-flight mass spectrometric（LC-TOF/MS） method was developed for the determination of 36 forbidden substances,belonging to β-agonists and anabolic hormones in feeds based on liquid chromatography-quadrupole/time-of-flight mass-spectrometry （LC-TOF/MS）.Acetonitrile and mixed sorbents were added to the homogeneous feeds sample,and then followed by the processing steps,involved vortexing dispersion,shaking extraction,centrifugation and concentration（namely the modified QuEChERS method）.The total analytes were rapidly extracted and purified.The extract was separated on a C18 column（150 mm×2.1 mm,2.7 μm） using methanol-0.1% formic acid as mobile phase by gradient elution,and analyzed under ESI positive ionization mode.Full scan experiments（TOF/MS ＆ Product ion） were performed over the m/z range of 100-1 000 Da.The quantitative analysis was carried out by extracting peak area with accurate mass.The confirmatory analysis of target compounds was performed with the qualitative fragments and retention time.Under the optimal conditions,a good separation and high sensitivity analysis of 36 substances were obtained with absolute value mass error below 7.3.The calibration curves were linear in the range of 10.0-200.0 μg/kg with correlation coefficients more than 0.99.The average recoveries at three spiked levels were in the range of 65%-120% with relative standard deviations （RSDs） no more than 24%.The proposed method was convenient,reliable and simple,and was suitable for the high-throughput and rapid screening analysis of forbidden drugs in feeds.