法医学杂志

法医学杂志 ›› 2018, Vol. 34 ›› Issue (6): 606-610.DOI: 10.12116/j.issn.1004-5619.2018.06.006

所属专题： 法医毒物学新技术

• 专题 • 上一篇    下一篇

人体尿液中卡西酮类毒品的SPE-GC-MS定性定量分析

王  平1，2，刘晓云1，2，3，刘  遥1，2，罗叶锋1，2，王  震1，2   

  1. 1. 广州正孚检测技术有限公司，广东 广州 510663； 2. 广东正孚法医毒物司法鉴定所，广东 广州 510663； 3. 广州万孚生物技术股份有限公司，广东 广州 510663
  • 发布日期:2018-12-25 出版日期:2018-12-28
  • 通讯作者: 刘晓云，女，博士，副主任法医师，主要从事法医毒物分析研究；E-mail：xyliu@wondfo.com.cn
  • 作者简介:王平（1989—），男，硕士研究生，主要从事法医毒物分析研究；E-mail：wnmc2007@163.com

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

WANG Ping1,2, LIU Xiao-yun1,2,3, LIU Yao1,2, LUO Ye-feng1,2, WANG Zhen1,2   

  1. 1. Guangzhou Accurate and Correct Test Company, Guangzhou 510663, China; 2. Guangdong Accurate and Correct Institution of Forensic Sciences, Guangzhou 510663, China; 3. Guangzhou Wondfo Biotech Co. Ltd., Guangzhou 510663, China
  • Online:2018-12-25 Published:2018-12-28

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摘要： 目的 建立人体尿液中卡西酮类毒品的固相萃取-气相色谱-质谱联用（solid phase extraction-gas chromatography-mass spectrometry，SPE-GC-MS）定性定量分析方法，并进行方法学验证。 方法 人体尿液样品经固相萃取法提取、七氟丁酸酐衍生后，通过气相色谱-质谱仪检测甲卡西酮、4-甲基甲卡西酮和3，4-亚甲二氧基甲卡西酮，采用内标法定量分析，从特异性、精密度、回收率等方面进行方法学验证。 结果 尿液中甲卡西酮、4-甲基甲卡西酮和3，4-亚甲二氧基甲卡西酮在25~200 ng/mL的质量浓度范围内线性良好（r>0.99），检出限均为2.0 ng/mL，定量限均为25.0 ng/mL，日内、日间精密度均小于6.0%，回收率为98.4%~105.7%。 结论 本研究所建立的方法准确性、特异性好，可以满足滥用药物人员尿液中卡西酮类毒品的定性定量分析，为卡西酮类滥用检测提供了技术保障。

关键词: 法医毒理学；固相萃取；气相色谱-质谱法；甲卡西酮；4-甲基甲卡西酮；3, 4-亚甲二氧基甲卡西酮；尿液

Abstract: Objective 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-N-methylcathinone showed good linearly in the range of 25-200 ng/mL of urine （r>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%. Conclusion The 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.

Key words: forensic toxicology, solid phase extraction, gas chromatography-mass spectrometry, methcathinone, 4-methyl methcathinone, 3,4-methylenedioxy-N-methylcathinone, urine