UPLC-ESIMS/MS法测定动物饲料中苯二氮卓类药物  

Determination of Benzodiazepines in Animal Feeds by UPLC-ESI MS/MS

作　　者：严丽娟[1] 张峰[2] 吴敏[1] 吴抒怀[1] 储晓刚[2] 周昱[1] 

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

出　　处：《分析测试学报》2011年第11期1301-1305,共5页Journal of Instrumental Analysis

基　　金：质检公益性行业科研专项课题(200910145);国家科技支撑计划项目(2009BADB9B02);厦门市科技计划项目(3502Z20092009;3502Z20112017)

摘　　要：建立了超高效液相色谱-电喷雾串联质谱(UPLC-ESI MS/MS)同时检测动物饲料中地西泮、奥沙西泮、硝西泮、三唑仑、艾司唑仑和咪达唑仑6种苯二氮卓类药物的方法。饲料样品采用碱性叔丁基甲醚提取,Oasis MCX固相萃取柱净化,反相色谱柱分离,以0.1%甲酸和乙腈为流动相进行梯度洗脱,正离子模式扫描,多反应监测模式检测,外标法定量。结果表明,6种苯二氮卓类药物在5～100μg/L范围内呈良好线性,方法的检出限为2μg/kg,定量下限为5μg/kg。在空白大猪配合饲料中添加5、20、100μg/kg 3个加标水平,6种药物的平均回收率为68%～94%,相对标准偏差为5.8%～12.7%。方法快速、准确、灵敏度高、重复性好,适用于动物饲料中苯二氮卓类药物的检测。An ultra-performance liquid chromatography - electrospray ionization tandem mass spectro etric （UPLC -ESI MS/MS） method was developed for the simultaneous determination of six benzodiazepines, including diazepam, oxazepam, nitrazepam, triazolam, estazolam and midazoalm, in animal feeds. The benzodiazepines in the feeds were extracted with alkaline tert-butyl methyl ether followed by clean-up with Oasis MCX cartridge. The LC separation was performed on a Waters Acquity UPLC BEH C,8 column（50 mm ×2. 1 mm, 1.7μm） by gradient elution using 0. 1% formic acid and acetonitrile as mobile phase at a flow rate of 0. 3 mL/min. The identification of six drugs was achieved by electrospray ionization tandem mass spectrometer under multiple reaction monitoring （MRM） mode and the quantification analysis was performed by the external standard method. The calibration curves showed good linearities in the range of 5 - 100 μg/L. The limits of detection （LOD） for the six drugs in feeds were 2 μg/kg and the limits of quantitation（LOQ） were 5 μg/kg. The average recoveries of the six drugs at three spiked levels of 5, 20, 100 μg/kg were between 68% and 94% with RSDs of 5.8% - 12.7%. The method was rapid, accurate and sensitive, and could be applicable in the routine assay on benzodiazepines in animal feeds.

关 键 词：苯二氮卓类 超高效液相色谱-串联质谱法 饲料 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]