色谱

色谱

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时快速确证检测血浆和尿液中的42种精神药物及其代谢产物

张秀尧*, 蔡欣欣, 张晓艺   

  1. 温州市疾病预防控制中心, 浙江 温州 325001
  • 收稿日期:2009-05-05 修回日期:2009-07-05 出版日期:2010-01-28 发布日期:1981-09-25
  • 通讯作者: 张秀尧

Rapid simultaneous determination of 42 psychoactive drugs and their metabolites in human plasma and urine by ultra performance liquid chromatography-tandem mass spectrometry

ZHANG Xiuyao*, CAI Xinxin, ZHANG Xiaoyi   

  1. Wenzhou Center for Disease Control and Prevention, Wenzhou 325001, China
  • Received:2009-05-05 Revised:2009-07-05 Online:2010-01-28 Published:1981-09-25
  • Contact: ZHANG Xiuyao

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941

被引次数

39

摘要： 针对公共卫生突发事件和临床毒物学检测实践中亟待解决的问题,建立了血浆和尿液中42种精神药物及其代谢产物的超高效液相色谱-串联质谱(UPLC-MS/MS)快速确证分析方法。样品经乙腈沉淀后,以乙酸铵和甲醇-乙腈(1:1, v/v)混合液作为流动相进行梯度洗脱,在Acquity UPLC BEH C18色谱柱上分离后用电喷雾串联质谱法检测,采用正、负离子快速切换多反应监测模式监测,基质标准同位素内标法定量。血浆样品中待测组分的加标回收率除了奋乃静、硫利哒嗪和氯丙嗪的分别为37.6%～57.5%, 36.3%～48.3%和52.4%～67.4%外,尿液样品中待测组分的加标回收率除了曲唑酮和地西泮的分别为100%～142%和108%～177%外,血浆和尿液中其余待测组分的加标回收率分别为60.2%～125%和64.5%～126%,相对标准偏差分别为0.8%～26%和2.6%～18%(n=6);除了巴比妥类药物的检出限为20～100 mg/L外,其余药物的检出限均为0.05～2.0 mg/L。该方法简单、快速、特异性强、灵敏度高。

关键词: 超高效液相色谱-串联质谱法, 精神药物, 尿液 , 确证, 血浆

Abstract: A rapid method for the simultaneous determination of 42 psychoactive drugs and their metabolites (barbitals, benzodiazepines, tricyclic antidepressants, phenothiazines, etc.) in human plasma and urine was developed using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). After a simple protein precipitation step, the analysis of the drugs and the metabolites was achieved on an Acquity UPLC BEH C18 column by using the gradient elution with ammonium acetate and methanol-acetonitrile (1:1, v/v) as the mobile phases, and detected by electrospray ionization-tandem mass spectrometry in the multiple reaction monitoring (MRM) mode operated simultaneously in both positive and negative modes by rapid switching, and quantified by matrix-match standard solution. The average recoveries were 60.2%~125% and 64.5%~126% for the drugs in plasma and urine except those of perphenazine, thioridazine and chloropromazine in plasma were 37.6%~57.5%, 36.3%~48.3%, 52.4%~67.4%, respectively; trazodone and diazepam in urine were 100%~142% and 108%~177%, respectively. The relative standard deviations (RSDs) of all the drugs in plasma and urine were within 0.8%~26% and 2.6%~18% (n=6), respectively. The detection limits of the 4 barbitals ranged from 20 to 100 mg/L and those of the other drugs ranged from 0.05 to 2.0 mg/L. The method is simple, selective and sensitive to detect drugs for both clinical and forensic purposes.

Key words: confirmation, plasma, psychoactive drugs, urine , ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)