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固相萃取/离子阱气相色谱质谱联用对血液中多种安眠药物的同时测定 被引量:19

Simultaneously Determination of Various Hypnotics in Human Blood by Solid-phase Extraction/Ion Trap Gas Chromatography-Mass Spectrometry
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摘要 建立了气相色谱-质谱联用测定血液中多种安眠药物的分析方法,通过固相萃取提取并富集血液样品中的9种常见巴比妥类、吩噻嗪类和苯二氮杂类安眠药物,采用离子阱二级质谱检测其含量。通过优化萃取溶液pH值及气相色谱-质谱联用分析条件,对9种安眠药物进行了定量分析。采用离子阱串联质谱(MS/MS)技术消除基底干扰,给出被测物结构信息。9种安眠药物的检出限为0.04~0.10 mg/L,回收率为78%~93%。方法用于人心血中安眠药物的检测,检出安定0.6 mg/L。该方法高效、简单、灵敏度高,可用于血液中巴比妥类、吩噻嗪类和苯二氮杂类安眠药物的同时测定。 A qualitative and quantitative analysis method was developed for determination of 9 hypnotics including barbiturates,phenothiazines and benzodiazepines by solid-phase extraction/ion trap gas chromatography-mass spectrometry.9 hypnotics in human blood were extracted and enriched by solid-phase extraction.The separation and quantitative analysis of 9 hypnotics was performed by ion trap gas chromatography-tandem mass spectrometry.pH values of extraction solution was optimized,and separation and detection conditions of gas chromatography-mass spectrometry were investigated.Tandem mass spectrometry technology was used to eliminate the interference of background,and provide structure information of the targeted compound by selecting characterization ions as parent ions.The result indicated that recoveries of 9 hypnotics ranged from 78% to 93%.The detection limits were in the range of 0.04-0.10 mg/L.The established method was applied in the quantitative analysis of blood from victim heart in criminal case and 0.6 mg/L diazepam was detected.The method was simple,high efficiency and sensitivity for the simultaneous determination of barbiturates,phenothiazines and benzodiazepines in human blood sample.
作者 陈建虎
出处 《分析测试学报》 CAS CSCD 北大核心 2010年第1期84-87,共4页 Journal of Instrumental Analysis
关键词 固相萃取 气相色谱质谱联用 血液 安眠药物 solid-phase extraction gas chromatography-mass spectrometry blood hypnotics
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