液相色谱-四极杆飞行时间质谱法筛查猪肉中5类26种药物残留  

Simultaneous Screening and Determination of Five Kinds of 26 Veterinary Drug Residues in Pork by Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry

作　　者：谢寒冰 王毅刚 周明莹[2] 赵海峰 蒋万枫 邓书 董诗竹 

机构地区：[1]青岛市"菜篮子"商品质量监督检测中心,山东青岛266071 [2]中国水产科学研究院黄海水产研究所,山东青岛266071

出　　处：《分析测试学报》2014年第4期373-379,共7页Journal of Instrumental Analysis

基　　金：青岛市2013年"菜篮子"工程建设资助项目

摘　　要：建立了同时筛查测定猪肉组织中氟喹诺酮类、磺胺类、有机磷类、β-激动剂类、四环素类5类26种药物残留的液相色谱-四极杆飞行时间质谱分析方法.试样采用QuEChERS前处理方法,样品经酸化乙腈-甲醇（1％乙酸,10％甲醇）提取.提取液以C18分散剂和正己烷净化,氮吹浓缩、定容后过滤膜上机检测.液相色谱以甲醇-水（0.1％甲酸）作为流动相梯度洗脱,C18色谱柱分离;高分辨质谱采用正离子模式检测,以二级质谱特征离子定性,以分子离子精确质量数提取色谱峰面积定量.结果表明26种药物的定量下限为0.4～10μg/kg;加标回收率为56.7％～106.2％,相对标准偏差（RSD）为7.7％～15.8％.方法操作简单、快速、高效,可作为猪肉中26种药物残留的快速筛查检测方法.A analytical method was established for the simultaneous screening and determination of 26 veterinary drugs, including 14 sulfonamides, 4/3-agonists, 2 flu0roquinolones, 3 tetracyclines and 3 organic phosphorus pesticides, in pork by liquid chromatography - quadrupole - time of flight mass spectrometry（HPLC- Q- TOF- MS）. The QuEChERS（Quick, Easy, Cheap, Effective, Rug- ged, and Safe） method was used for sample preparation. The samples were extracted with acidified acetonitrile- methanol（ 1% acetic acid, 10% methanol）, and cleaneded up by dispersive solid- phase extraction using C18 dispersant sorbent, then degreased with hexane. The 26 veterinary drugs were separated on an Eclipse Plus C18 （3.0 mm x 100 mm, 1.8 μm） column using water with 0. 1% formic acid（A） and methanol（B） as mobile phase by gradient elution in 19 min, and analyzed by MS under ESI positive ionization mode. The quantitation analysis was carried out by extracting peak area with accurate mass. The confirmatory analysis of target compounds was performed with the quali- tative fragments. The results showed that the limits of quantitation （ LOQ, S/N = 10） of 26 target compounds in pork ranged from 0. 4 μg/kg to 10 μg/kg. The mean recoveries of 26 veterinary drugs were in the range of 56.7% - 106. 2% , with RSDs of 7.7% - 15.8%. With the advantages of sim- plicity, fast, efficient, the method was suitable for the analysis of 26 veterinary drugs in pork.

关 键 词：液相色谱-四极杆飞行时间质谱 猪肉 兽药 多残留 快速筛查 high performance liquid chromatography-tandem mass spectrometry(HPLC-Q-TOF-MS) 

分 类 号：I657.63[文学—其他各国文学] TQ645.1[化学工程—精细化工]