超高效液相色谱-串联质谱法同时测定畜禽产品中15种镇静类药物残留

Determination of 15 Sedative Drugs Residues in Livestock and Poultry Meat by UPLC-MS/MS

建立了超高效液相色谱串联质谱法(UPLC-MS/MS)快速测定畜禽产品中15种镇静类药物残留的方法。样品用乙腈-乙酸乙酯溶液提取,提取液经二乙烯苯/N-乙烯基吡咯烷酮共聚物分散固相萃取净化,反萃浓缩后测定,以0.1%甲酸水-0.1甲酸乙腈作为流动相进行梯度洗脱,在Poroshell 120 EC-C_(18)(100 mm L×2.1 mm ID,2.7μm)色谱柱上分离,柱温35℃,流速0.3 m L/min,进样量5μL,在电喷雾正离子模式下以动态多反应监测(Dynamic MRM)采集数据,外标法定量。结果表明,15种镇静类药物在各自质量浓度范围内线性较好,相关性系数R2≥0.999,于不同基质中(牛肉、鸡肉、猪肝)进行高、中、低浓度水平的加标试验回收率为74.1%~88.2%,相对标准偏差(RSD)为2.9%~8.5%,方法检出限(LOD,S/N≥3)为1.0~2.0μg/kg,定量限为3.0~6.0μg/kg。经方法学考查,该方法简单快速、灵敏度高、重现性好、结果准确,适用于畜禽产品中15种镇静类药物的定性筛查和准确定量。

A method for rapid determination of residues of 15 sedative drugs in poultry meat was developed.The sample was extracted with acetonitrile-acetic acid ethyl ester solution,and the extraction solution after salting was purified by HLB dispersed solid phase extraction,and then determined after backextraction and concentration.Data were collected by Dynamic multi-reaction monitoring(Dynamic MRM)in electrospray cation mode with a sample size of 5μL,flow rate of 0.3 mL/min,mobile phase of 0.1%water-formic and acetonitrile,a column of Poroshell 120 EC-C18(100 mmL×2.1 mm ID,2.7μm)and the column temperature of 35℃.The analytes were quantitated by external standard method.Statistics indicated that this method whose RSD was 2.9%~8.5%,had a good linear with R2≥0.999 in their ranges of linearity,what's more,the LODs of which were 1.0~2.0μg/kg and the LOQs were 3.0~6.0μg/kg along with a hige recovery rate ranged 74.1%~88.2%from different sample matrixes(beef,chicken,pork liver)added 3 levels of concentration.In a word,it was suitable for rapid screening and quantitative determination of 15 sedative drugs in livestock and poultry meat.