超高效液相色谱-四极杆飞行时间质谱快速检测动物饲料中10种违禁精神药物

Simultaneous determination of 10 unapproved sedative drugs in feeds by ultra-performance liquid chromatographyquadrupole-time-of-flight mass spectrometry

建立了测定动物饲料中三唑仑、艾司唑仑、硝西泮、地西泮、异丙嗪、氯氮平、唑吡坦、甲硫哒嗪、氯丙嗪和咪达唑仑10种违禁精神药物的超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF-MS)方法。样品经混合溶剂甲醇-0.1 mo l/L HCl(9∶1,v/v)振荡提取,再用MCX固相萃取柱净化处理后,采用UPLC-Q-TOF-MS分析检测。10种化合物在5～100μg/L范围内均呈良好的线性关系,线性相关系数均大于0.99。本方法的硝西泮、唑吡坦和甲硫哒嗪的定量限(LOQ,以信噪比为10计)为8μg/kg,三唑仑、艾司唑仑、地西泮、异丙嗪、氯丙嗪和咪达唑仑为10μg/kg,氯氮平为20μg/kg。3个添加水平(LOQ、2LOQ、4LOQ)的回收率试验结果表明,10种化合物的回收率在60.6%～108.5%范围内,相对标准偏差均小于10%。本方法可用于动物饲料中违禁精神药物的准确测定。

A new analytical method using ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry（UPLC-Q-TOF-MS） was developed for screening and confirmation of 10 unapproved sedative drugs in feeds.The samples were extracted using the solution of methanol-0.1 mol/L HCl（9∶1,v/v）,and the extracts were centrifuged and then directly purified through MCX cartridges.The identification and detection were achieved in positive electrospray ionization（ESI） mode using Q-TOF-MS.The potential of UPLC-Q-TOF MS for confirmatory analysis was shown by determining the accurate mass of all the compounds and fragment ions upon collision-induced-dissociation（CID） at different energies.The extra mass measurement errors for all the sedative drugs were found to be within 5 ppm.The calibration graphs were linear in the concentration range of 5-100 μg/L with the correlation coefficients more than 0.99 for the 10 drugs.The limits of quantification（LOQ,S/N=10） were 8 μg/kg for nitrazepam,zolpidem and thioridazine;10 μg/kg for thriazolam,estazolam,diazepam,promethazine,chlorpromazine and midazolam;20 μg/kg for clozapine.The recoveries for all the compounds in feeds were 60.6%-108.5% with the relative standard deviations less than 10% at the spiked levels of LOQ,2LOQ and 4LOQ.