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快速溶剂萃取-气相色谱-串联质谱法测定血中巴比妥类药物 预览 被引量:8

GC-MS/MS Determination of Barbiturate Drugs in Blood with Accelerated Solvent Extraction
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摘要 提出了气相色谱-串联质谱法测定血中巴比妥类药物(巴比妥、苯巴比妥、异戊巴比妥、司可巴比要)含量的方法。样品以乙酸乙酯-环己烷(1+1)混合液为萃取剂,经快速溶剂萃取仪提取后,提取液用氮气吹干后以1.0mL甲醇溶解,通过VF-5MS色谱柱分离,采用电子轰击离子源多反应监测模式进行质谱测定。4种巴比妥类药物的质量浓度与其峰面积均在10~1000μg·L^-1之间呈线性关系,检出限(3S/N)在0.07~0.26μg·L^-1之间。以空白血液样品为基体进行回收试验,测得回收率在77.8%~93.4%之间,测定值的相对标准偏差(n=7)在2.3%~6.9%之间。 GC-MS/MS was applied to the determination of barbiturate drugs, i. e. , barbital, amobarbital, secobarbital and phenobarbital, in blood. The sample was extracted with a mixture of ethyl acetate and cyclohenane (1+1) by accelerated solvent extraction, and the extract was evaporated to dryness by N2-blowing and dissolved with 1. 0 mL of methanol. VF-5MS chromatrographic column was used for separation, and the multi-reactions monitoring with electron impact ionization source was adopted in MS. Linear relationships between values of peak area and mass concentration of the 4 barbiturate drugs were kept in the same range of 10- 1 000 μg . L^-1, with detection limits (3S/N) in the range of 0.07--0. 26 μg. L^-1. On the base of blank blood sample, test for recovery was made by standard addition method, values of recovery found were in the range of 77.8%-93.4%, with RSD% (n=7) in the range of 2.3%-6.9%.
作者 唐磊 应剑波 TANG Lei, YING Jian-bo (Institute of Criminal Science and Technology, Hangzhou Municipal Public Security Bureau, Hangzhou 310004, China)
出处 《理化检验:化学分册》 CAS CSCD 北大核心 2012年第7期845-847,850共4页 Physical Testing and Chemical Analysis Part B:Chemical Analgsis
基金 公安部重点研究计划项目(2010ZDYJZJST013)
关键词 气相色谱-串联质谱法 快速溶剂萃取 巴比妥 苯巴比妥 异戊巴比妥 司可巴比妥 C,C-MS/MS Accelerated solvent extraction~ Blood Barbital Phenobarbital~ AmobarbitalSecobarbital
作者简介 唐磊(1982-),男,浙江富阳人,硕士,助理工程师,主要从事毒物分析。E-mail:ta1911@163.com
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