Determination of Common Drugs and Metaboliteies in Hair by UHPLC-MS/MS with Ultrasonic Extraction
摘 要
建立了超声提取-超高效液相色谱-串联质谱法(UHPLC-MS/MS)测定毛发中常见毒品及代谢物含量的方法。称取洗涤(水、二氯甲烷、丙酮依次振荡洗涤各1次)并晾干后的毛发样品40~60 mg,将其剪成约1 mm小段,加入3.2 mm的破碎珠6颗,冷冻破碎5 min;再称取破碎后的毛发样品20 mg,加入1 mL甲醇,于0℃冰水浴中超声提取20 min,上清液用0.25 μm有机滤膜过滤,滤液供UHPLC-MS/MS测定。结果显示:O6-单乙酰吗啡(6-AM)、吗啡(MOR)、氯胺酮(K粉)、甲基苯丙胺(MAMP)、苯丙胺(AMP)、可卡因(COC)、苯甲酰爱康宁(BZE)、3,4-亚甲双氧甲基苯丙胺(MDMA)、3,4-亚甲双氧苯丙胺(MDA)、3,4-亚甲双氧乙基苯丙胺(MDEA)、可待因(COD)、去甲氯胺酮(NK)、Δ9-四氢大麻酚(THC)、大麻二酚(CBD)、大麻酚(CBN)等15种目标物的质量分数在一定范围内与其对应的峰面积呈线性关系,BZE、THC、CBD、COC、CBN的检出限(3S/N)均为0.001 ng·mg-1,6-AM、MOR、K粉、MAMP、AMP、MDMA、MDA、MDEA、COD、NK的检出限(3S/N)均为0.004 ng·mg-1;按照标准加入法对3个浓度水平的空白样品溶液进行测定,回收率为73.3%~97.8%,测定值的相对标准偏差(RSD,n=10)为4.3%~14%。方法用于实际样品的检测,测定结果与司法鉴定技术规范的测定结果一致。
Abstract
A method for determination of common drugs and metabolites in hair by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) with ultrasonic extraction was established. Hair sample of 40-60 mg was dried after washing by water, dichlorocarbon and acetone. The hair sample was cut into 1 mm segments, and 6 broken beads of 3.2 mm were added. The sample was broken cryogenically for 5 min. Then methanol of 1 mL was added into broken hair sample of 20 mg, and ultrasonic extraction was carried out at 0℃ for 20 min in an ice-water bath. The supernatant was filtered by 0.25 μm organic filter membrane and determined by UHPLC-MS/MS. It was showed that linear relationships between mass fractions of O6-monoacetylmorphine (6-AM), morphine (MOR), ketamine, methamphetamine (MAMP), amphetamine (AMP), cocaine (COC), benzoyl-iconine (BZE), 3,4-methylene dioxymethamphetamine (MDMA), 3,4-methylene dioxyamphetamine (MDA), 3,4-methylene dioxyethyl amphetamine (MDEA), codeine (COD), normethylene ketamine (NK), tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN) and their peak areas were kept in definite ranges, with detection limits (3S/N) of 0.001 ng·mg-1 for BZE, THC, CBD, COC, CBN, and 0.004 ng·mg-1 for 6-AM, MOR, ketamine, MAMP, AMP, MDMA, MDA, MDEA, COD, NK. Recovery test was made on blank samples at 3 concentration levels by standard addition method, giving results in the range of 73.3%-97.8%, and RSDs (n=10) of the determined values were ranged from 4.3% to 14%. This method has been used to test substantial samples, and the results were consistent with those of standards of forensic science.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202201010
所属栏目 工作简报
基金项目 贵州省高层次“百”层次创新型人才项目(黔科合平台人才[2020]6012);贵州省科技计划项目(黔科合支撑[2019]2825号、黔科合支撑[2020]4Y057号);贵州省大学生创新创业训练计划项目(S202010660017);贵州省大学生创新创业训练计划项目(399);贵州省高技术产业化示范工程项目(黔发改高技[2016]1345号)
收稿日期 2020/6/24
修改稿日期
网络出版日期
作者单位点击查看
备注陈顺琴,硕士,研究方向为毒(药)物学
引用该论文: CHEN Shunqin,TANG Mei,HUANG Jiang,WANG Jie,WANG Aimin,ZHU Faze,LIU Yubo,LUO Peng. Determination of Common Drugs and Metaboliteies in Hair by UHPLC-MS/MS with Ultrasonic Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(1): 58~64
陈顺琴,唐美,黄江,王杰,王爱民,朱发泽,刘玉波,罗鹏. 超声提取-超高效液相色谱-串联质谱法测定毛发中常见毒品及代谢物的含量[J]. 理化检验-化学分册, 2022, 58(1): 58~64
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】杨洪国,李重阳,丁斌.毒品与毛发的结合及其影响因素[J].中国司法鉴定, 2013(1):46-49.
【2】KINTZ P. Issues about axial diffusion during segmental hair analysis[J]. Therapeutic Drug Monitoring, 2013,35(3):408-410.
【3】SELDōN T, BERGLUND L, DRUID H, et al. O9:Segmental hair analysis from patients in opiate substitution treatment is useful to investigate drug use history, abstinence and compliance with treatment[J]. Toxicologie Analytique et Clinique, 2014,26(2):8-9.
【4】韩军,李纬,李彬,等.毛发中痕量毒品快速检测技术解析[J].警察技术, 2019(4):82-84.
【5】刘缙,蔡红新,钱斌,等.分散液液微萃取预处理-气相色谱-质谱法快速测定人尿中3种毒品方法改进[J].理化检验-化学分册, 2019,55(12):1442-1447.
【6】SHU I, ALEXANDER A, JONES M, et al. Determination of methamphetamine enantiomer composition in human hair by non-chiral liquid chromatography-tandem mass spectrometry method[J]. Journal of Chromatography B, 2016,1028:145-152.
【7】杨崇俊,李强,高中勇,等.HS-SPME-GC/MS法检测尿液及毛发中苯丙胺类毒品[J].中国法医学杂志, 2014,29(2):93-96.
【8】WANG M, CHENG C S, LIU C B, et al. Hollow fiber supported ionic liquids liquid-phase micro-extraction followed by high-performance liquid chromatography for the determination of polycyclic aromatic hydrocarbons in milk samples[J]. Journal of Chromatographic Science, 2018,56(1):74-80.
【9】杨崇俊,张红丽,李强,等.高动能研磨-液质法快速检测毛发中毒品及其代谢物[J].分析试验室, 2019,38(5):604-608.
【10】ORFANIDIS A, MASTROGIANNI O, KOUKOU A, et al. A GC-MS method for the detection and quantitation of ten major drugs of abuse in human hair samples[J]. Journal of Chromatography B, 2017,1047:141-150.
【11】王伟,徐唯哲,李清艳.人毛发中吗啡类毒品的色谱检测方法文献分析[J].中国法医学杂志, 2018,33(4):401-405.
【12】朱丹,孟品佳,路春清.动态液相微萃取GC/MS-SIM方法检验毛发中的苯丙胺类毒品[J].分析试验室, 2007,26(7):57-60.
【13】国菲,王燕燕,孟品佳,等.海洛因滥用者毛发中毒品代谢物的固相萃取-GC/MS分析[J].分析试验室, 2010,29(2):121-124.
【14】任冠恒,燕启江,唐鹰,等.人毛发中苯丙胺类毒品检测方法的研究进展[J].法医学杂志, 2019,35(1):89-94.
【15】BOUMBA V A, DI RAGO M, PEKA M, et al. The analysis of 132 novel psychoactive substances in human hair using a single step extraction by tandem LC/MS[J]. Forensic Science International, 2017,279:192-202.
【16】CHEONG J C, SUH S, KO B J, et al. Screening method for the detection of methamphetamine in hair using fluorescence polarization immunoassay[J]. Journal of Analytical Toxicology, 2013,37(4):217-221.
【17】中华人民共和国司法部公共法律服务管理局.毛发中15种毒品及代谢物的液相色谱-串联质谱检验方法:SF/Z JD0107025-2018[S].北京:中国标准出版社, 2018.
【18】中华人民共和国司法部司法鉴定管理局.生物检材中单乙酰吗啡、吗啡、可待因的测定:SF/Z JD0107006-2010[S].北京:中国标准出版社, 2010.
【19】中华人民共和国司法部司法鉴定管理局.生物检材中苯丙胺类兴奋剂、哌替啶和氯胺酮的测定:SF/Z JD0107004-2016[S].北京:中国标准出版社, 2016.
【2】KINTZ P. Issues about axial diffusion during segmental hair analysis[J]. Therapeutic Drug Monitoring, 2013,35(3):408-410.
【3】SELDōN T, BERGLUND L, DRUID H, et al. O9:Segmental hair analysis from patients in opiate substitution treatment is useful to investigate drug use history, abstinence and compliance with treatment[J]. Toxicologie Analytique et Clinique, 2014,26(2):8-9.
【4】韩军,李纬,李彬,等.毛发中痕量毒品快速检测技术解析[J].警察技术, 2019(4):82-84.
【5】刘缙,蔡红新,钱斌,等.分散液液微萃取预处理-气相色谱-质谱法快速测定人尿中3种毒品方法改进[J].理化检验-化学分册, 2019,55(12):1442-1447.
【6】SHU I, ALEXANDER A, JONES M, et al. Determination of methamphetamine enantiomer composition in human hair by non-chiral liquid chromatography-tandem mass spectrometry method[J]. Journal of Chromatography B, 2016,1028:145-152.
【7】杨崇俊,李强,高中勇,等.HS-SPME-GC/MS法检测尿液及毛发中苯丙胺类毒品[J].中国法医学杂志, 2014,29(2):93-96.
【8】WANG M, CHENG C S, LIU C B, et al. Hollow fiber supported ionic liquids liquid-phase micro-extraction followed by high-performance liquid chromatography for the determination of polycyclic aromatic hydrocarbons in milk samples[J]. Journal of Chromatographic Science, 2018,56(1):74-80.
【9】杨崇俊,张红丽,李强,等.高动能研磨-液质法快速检测毛发中毒品及其代谢物[J].分析试验室, 2019,38(5):604-608.
【10】ORFANIDIS A, MASTROGIANNI O, KOUKOU A, et al. A GC-MS method for the detection and quantitation of ten major drugs of abuse in human hair samples[J]. Journal of Chromatography B, 2017,1047:141-150.
【11】王伟,徐唯哲,李清艳.人毛发中吗啡类毒品的色谱检测方法文献分析[J].中国法医学杂志, 2018,33(4):401-405.
【12】朱丹,孟品佳,路春清.动态液相微萃取GC/MS-SIM方法检验毛发中的苯丙胺类毒品[J].分析试验室, 2007,26(7):57-60.
【13】国菲,王燕燕,孟品佳,等.海洛因滥用者毛发中毒品代谢物的固相萃取-GC/MS分析[J].分析试验室, 2010,29(2):121-124.
【14】任冠恒,燕启江,唐鹰,等.人毛发中苯丙胺类毒品检测方法的研究进展[J].法医学杂志, 2019,35(1):89-94.
【15】BOUMBA V A, DI RAGO M, PEKA M, et al. The analysis of 132 novel psychoactive substances in human hair using a single step extraction by tandem LC/MS[J]. Forensic Science International, 2017,279:192-202.
【16】CHEONG J C, SUH S, KO B J, et al. Screening method for the detection of methamphetamine in hair using fluorescence polarization immunoassay[J]. Journal of Analytical Toxicology, 2013,37(4):217-221.
【17】中华人民共和国司法部公共法律服务管理局.毛发中15种毒品及代谢物的液相色谱-串联质谱检验方法:SF/Z JD0107025-2018[S].北京:中国标准出版社, 2018.
【18】中华人民共和国司法部司法鉴定管理局.生物检材中单乙酰吗啡、吗啡、可待因的测定:SF/Z JD0107006-2010[S].北京:中国标准出版社, 2010.
【19】中华人民共和国司法部司法鉴定管理局.生物检材中苯丙胺类兴奋剂、哌替啶和氯胺酮的测定:SF/Z JD0107004-2016[S].北京:中国标准出版社, 2016.
相关信息