固相萃取-超高效液相色谱-串联质谱法同时测定猪肉中20种精神药物残留  

Simultaneous determination of twenty psychoactive drugs in pork bysolid phase extraction coupled with ultra performance liquid chromatographytandem mass spectrometry

作　　者：孙婷[1] 王鹭骁[1] 曾三妹[1] 吴敏[1] 严丽娟[1] 张峰[2] 黄志强[3] 

机构地区：[1]厦门出入境检验检疫局,福建厦门361012 [2]中国检验检疫科学研究院,北京100025 [3]湖南出入境检验检疫局,湖南长沙410004

出　　处：《色谱》2014年第7期702-706,共5页Chinese Journal of Chromatography

基　　金：国家科技支撑计划项目(2009BADB9B02;2012BAK08B01);国家重大科学仪器设备开发专项项目(2012YQ14000806)

摘　　要：建立了固相萃取和超高效液相色谱-电喷雾串联质谱（UPLC-ESI-MS/MS）同时测定猪肉中20种精神药物残留的方法。样品采用碱性乙腈作为提取试剂,提取液经Oasis MCX固相萃取柱净化后,以含0.1%（v/v）甲酸的水溶液和乙腈作为流动相梯度洗脱,用C18色谱柱分离,正离子模式扫描,多反应监测模式检测。20种化合物在5-100μg/L质量浓度范围内均呈良好的线性关系,线性相关系数均大于0.99,以S/N≥10计算方法的定量限为5μg/kg。在空白猪肉中添加5、10和50μg/kg水平的20种药物,其平均回收率为66.8%-97.2%,相对标准偏差（RSD）为4.2%-12.4%。本方法快速、准确、可靠,适用于猪肉中精神药物多残留的同时测定。A method for the simultaneous determination of 20 psychoactive drugs in pork by solid phase extraction coupled with ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry（UPLC-ESI-MS/MS）was established.The samples were extracted with alkalified acetonitrile,and then cleaned up using solid phase extraction with an Oasis MCX column.The UPLC separation was performed on a C18 column（50 mm×2.1 mm,1.7μm）using agradient elution with the mobile phases of 0.1%（v/v）formic acid in water and acetonitrile.The ESIMS/MS detection was achieved in positive mode under multiple reaction monitoring（MRM）mode.The calibration curves showed good linearity in the range of 5-100μg/L with the correlation coefficients more than0.99 for the 20 psychoactive drugs.The limits of quantification（LOQ,S/N≥10）for the 20 psychoactive drugs were 5μg/kg.The average recoveries of the 20 psychoactive drugs spiked in blank pork at three levels of 5,10 and50μg/kg were 66.8%-97.2% with the relative standard deviations from4.2%to 12.4%.The method is suitable for the simultaneous determination of the 20 psychoactive drugs in pork with the characteristics of easy operation,high accuracy and precision.

关 键 词：固相萃取 超高效液相色谱-电喷雾串联质谱 精神药物 猪肉 

分 类 号：O658[理学—分析化学]