中空纤维膜液相微萃取-气相色谱/三重四级杆质谱法检测尿液和血液样品中8种毒品  

Hollow Fiber Liquid-Phase Microextraction for the Determination of Drugs of Abuse in Urine and Blood Samples by Gas Chromatography-Triple Quadrupole Mass Spectrometry

作　　者：孟梁[1] 张文文 朱彬玲[1] 郑可芳[1] 

机构地区：[1]福建警察学院刑事科学技术系,福建福州350007 [2]北京市公安局公安交通管理局,北京100037

出　　处：《分析科学学报》2016年第3期366-370,共5页Journal of Analytical Science

基　　金：福建省教育厅中青年教师教育科研基金(No.JA14336)

摘　　要：建立了生物样品尿液和血液中8种毒品的中空纤维膜液相微萃取-气相色谱/三重四级杆质谱检测方法。对影响萃取富集效率的因素通过正交试验进行优化,确定最佳条件如下:选择甲苯作为萃取剂,在样品溶液pH=13.0的条件下用5cm长的中空纤维膜进行萃取,萃取温度为30℃,搅拌速度为600r·min^(-1)。萃取后抽取有机溶剂供气相色谱/三重四级杆质谱分析检测。结果表明,各分析物在0.0003~10μg·mL^(-1)范围具有良好的线性关系,线性相关系数R在0.9985~0.9995之间;检出限(S/N=3)为0.05~0.5ng·mL^(-1);样品加标回收率在79.3%~98.6%之间,相对标准偏差(RSD)<4.5%(n=5)。该方法具有净化能力好、操作简单、灵敏度高和重现性好等优点,能用于生物样品中多种毒品的高灵敏度分析检测。The hollow fiber liquid-phase microextraction（HF-LPME）was applied for the determination of multiple drugs of abuse in urine and blood samples by gas chromatography-triple quadrupole mass spectrometry（GC-QQQ-MS）.Parameters affecting extraction efficiency were investigated and optimized.Toluene was chosen as the extractant and held by 5cm of hollow fiber for liquid-phase microextraction.The pH of sample solution was 13.0.The extracting temperature was 30℃.The stirring rate was 600r·min-1.Under the optimum conditions,linearities were observed for all analytes in the range from 0.0003 to 10 μg·mL-1 with the correlation coefficients（R）ranging from 0.9985 to 0.9995.The recoveries of 79.3%-98.6% with relative standard derivations〈4.5%（n=5）were obtained.The limits of detection were estimated to be in the range from 0.05 to 0.5ng·mL-1（S/N=3）.The technique showed the advantages of higher purifying capacity,less extraction time,and higher extraction efficiency.It was successfully applied to the analysis of amphetamines in real human blood sample.

关 键 词：中空纤维膜 液相微萃取 气相色谱/三重四级杆质谱 毒品 生物样品 

分 类 号：O657.63[理学—分析化学]