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固相萃取-气相色谱-质谱联用法定性定量分析人尿液中的卡西酮类物质

Qualitative and Quantitative Analysis of Cathinones in Human Urine by SPE-GC-MS.

作者信息

Wang P, Liu X Y, Liu Y, Luo Y F, Wang Z

机构信息

Guangzhou Accurate and Correct Test Company, Guangzhou 510663, China.

Guangdong Accurate and Correct Institution of Forensic Sciences, Guangzhou 510663, China.

出版信息

Fa Yi Xue Za Zhi. 2018 Jun;34(6):606-610. doi: 10.12116/j.issn.1004-5619.2018.06.006. Epub 2018 Dec 25.

DOI:10.12116/j.issn.1004-5619.2018.06.006
PMID:30896097
Abstract

OBJECTIVES

To propose an alternative solid phase extraction-gas chromatography-mass spectrometry (SPE-GC-MS) method for the sensitive determination of cathinones in human urine samples, plus methodological verification.

METHODS

Human urine samples were concentrated by solid phase extraction (SPE) sorbent and converted into the corresponding heptafluorobutyric acid anhydride derivatives. Methcathinone, 4-methyl methcathinone and 3,4-methylenedioxy-N-methylcathinone were detected by gas chromatography-mass spectrometry (GC-MS). With quantitative analysis by internal standard method, methodological verification was carried out from the aspects of specificity, precision and reco-very rate.

RESULTS

Methcathinone, 4-methyl methcathinone and 3,4-methylenedioxy--methylcathinone showed good linearly in the range of 25-200 ng/mL of urine (>0.99), with the limits of detection 2.0 ng/mL, limit of quantitation 25.0 ng/mL, both intra- and inter-day coefficients of variation lower than 6.0%, and recovery rates of 98.4%-105.7%.

CONCLUSIONS

he proposed SPE-GC-MS procedure has good accuracy and specificity, can meet the need of qualitative and quantitative analysis of cathinones in the urine of drug abusers, and therefore provide technical support for the detection of cathinone abuse.

摘要

目的

提出一种用于灵敏测定人尿液样本中卡西酮的固相萃取-气相色谱-质谱联用(SPE-GC-MS)替代方法,并进行方法学验证。

方法

人尿液样本通过固相萃取(SPE)吸附剂进行浓缩,并转化为相应的七氟丁酸酐衍生物。通过气相色谱-质谱联用(GC-MS)检测甲基卡西酮、4-甲基甲基卡西酮和3,4-亚甲基二氧基-N-甲基卡西酮。采用内标法进行定量分析,从特异性、精密度和回收率等方面进行方法学验证。

结果

甲基卡西酮、4-甲基甲基卡西酮和3,4-亚甲基二氧基-N-甲基卡西酮在尿液浓度为25-200 ng/mL范围内呈良好线性关系(>0.99),检测限为2.0 ng/mL,定量限为25.0 ng/mL,日内和日间变异系数均低于6.0%,回收率为98.4%-105.7%。

结论

所提出的SPE-GC-MS方法具有良好的准确性和特异性,能够满足吸毒者尿液中卡西酮定性和定量分析的需求,为卡西酮滥用检测提供技术支持。

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