色谱

色谱 ›› 2012, Vol. 30 ›› Issue (05): 457-462.DOI: 10.3724/SP.J.1123.2011.12032

• 研究论文 • 上一篇    下一篇

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

许成保1, 2, 锁然1*, 张峰2*, 储晓刚2, 丁菲2, 3, 凌云2, 杨敏莉2, 孙利2   

  1. 1. 河北农业大学, 河北 保定 071001; 2. 中国检验检疫科学研究院, 北京 100123; 3. 浙江中医药大学, 浙江 杭州 310053
  • 收稿日期:2011-12-14 修回日期:2012-02-13 出版日期:2012-05-28 发布日期:2012-06-07
  • 通讯作者: 锁然,博士,副教授,主要从事食品有害物检测方面的教学研究. E-mail: xuchengbao123@126.com.张 峰,博士,副研究员,主要从事色谱和质谱等方面的检验检疫研究. E-mail: fengzhang@126.com.
  • 基金资助:

    国家科技支撑计划项目(批准号: 2009BADB9B02)、质量检验公益性行业科研项目(批准号: 200910145)、国家质量监督检验检疫总局科技计划项目(批准号: 2008IK167)和北京市科技计划项目(批准号: D08050200310803).

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

XU Chengbao1,2, SUO Ran1*, ZHANG Feng2*, CHU Xiaogang2, DING Fei2,3, LING Yun2, YANG Minli2, SUN Li2   

  1. 1. Agricultural University of Hebei, Baoding 071001, China; 2. Chinese Academy of Inspection and Quarantine, Beijing 100123, China; 3. Zhejiang Chinese Medical University, Hangzhou 310053, China
  • Received:2011-12-14 Revised:2012-02-13 Online:2012-05-28 Published:2012-06-07

PDF

328

被引次数

31

摘要： 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 mol/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5～100 μg/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8 μg/kg,三唑仑、艾司唑仑、地西泮、异丙嗪、氯丙嗪和咪达唑仑为10 μg/kg,氯氮平为20 μg/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。

关键词: 超高效液相色谱-四极杆飞行时间质谱, 饲料, 违禁精神药物

Abstract: 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.

Key words: feeds, unapproved sedative drugs, ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS)

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