高效液相色谱-串联质谱法检测新型毒品中的合成大麻素
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摘要
目的建立新型毒品中合成大麻素定性、定量分析的高效液相色谱-三重四极杆质谱检测方法。方法样品经甲醇超声提取后,离心,取上清液过膜(0.22μm),采用Agilent Poroshell 120 EC-C 18 (4.6mm×100mm,2.7μm)色谱柱,以含0.1%甲酸的乙腈-水为流动相进行梯度洗脱,流速0.6mL/min。质谱的检测采用电喷雾电离-正离子、动态MRM的检测模式。结果该方法实现了对8种常见合成大麻素定性和定量分析,各化合物在0.5～500ng/mL范围内具有良好的线性关系,最低检出限在0.01～0.1ng/mL范围内,日内相对标准偏差均不大于3.05%,日间相对标准偏差均不大于5%。结论本文建立的方法具有快速、灵敏、准确、可靠等优点,适用于相关案件中合成大麻素类新型毒品的检验鉴定。
Objective To establish a method for detecting synthetic cannabinoids in novel drugs by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). Methods The samples were extracted by methanol with ultrasound and then centrifuged, having left the supernatant to be ?ltered through the 0.22μm membrane. The ?ltrate was separated through an Agilent Poroshell 120 EC-C 18(4.6×100 mm, 2.7μm) column(insetting into Agilent 1200 in?nity LC apparatus) by a gradient elution at a ?ow rate of 0.6 mL/min running with the mobile phase of hydro-acetonitrile solvent containing 0.1% formic acid. ESI(+), combining with the dynamic MRM mode, was used to detect the eluted synthetic cannabinoids. Results Eight common synthetic cannabinoids were carried out of their qualitative and quantitative analysis, all showing a good linear relationship in the range of 0.5-500 ng/mL and the low detection limit ranging among 0.01-0.1 ng/mL.The RSDs of intra-and inter-day were less than 3.05% and 5%, respectively. Conclusions The method presented here is rapid,sensitive and accurate, suitable for the identi?cation of synthetic cannabinoids in novel drugs involving into narcotic-abusing cases.
Objective To establish a method for detecting synthetic cannabinoids in novel drugs by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). Methods The samples were extracted by methanol with ultrasound and then centrifuged, having left the supernatant to be ?ltered through the 0.22μm membrane. The ?ltrate was separated through an Agilent Poroshell 120 EC-C 18(4.6×100 mm, 2.7μm) column(insetting into Agilent 1200 in?nity LC apparatus) by a gradient elution at a ?ow rate of 0.6 mL/min running with the mobile phase of hydro-acetonitrile solvent containing 0.1% formic acid. ESI(+), combining with the dynamic MRM mode, was used to detect the eluted synthetic cannabinoids. Results Eight common synthetic cannabinoids were carried out of their qualitative and quantitative analysis, all showing a good linear relationship in the range of 0.5-500 ng/mL and the low detection limit ranging among 0.01-0.1 ng/mL.The RSDs of intra-and inter-day were less than 3.05% and 5%, respectively. Conclusions The method presented here is rapid,sensitive and accurate, suitable for the identi?cation of synthetic cannabinoids in novel drugs involving into narcotic-abusing cases.
引文
[1]SEBASTIAN D,STEFAN K,WOLFGANG W,et al.Develop-ment and validation of a liquid chromatography-tandem mass spectrometry method for the quartitation of synthetic cannabi-noids of the aminoalkylindole type and methanandamide in se-rum and its application to forensic samples[J].Journal of Mass Spectrometry.2011,46:163-171.
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[3]梁晨,郑水庆,陈永生,等.检出新型毒品K2一例[J].中国司法鉴定,2011(5):S13-S14.
[4]徐鹏,刘克林,钱振华.首例“Peace Out”香料的GC/MS检验[J].中国药物滥用防治杂志,2012,18(2):120-123.
[5]李茂盛,郑水庆,陈永生,等.GC-MS检测新型策划毒品K3[J].中国司法鉴定,2013,(5):20-23.
[6]EMCDDA.Thematic papers:understanding the“Spice”phe-nomenon[M].Lisbon:European Monitoring Centre for Drugs and Drug Addiction(EMCDDA),2009.
[7]LANGER N,LINDIGKEIT R,SCHIEBEL N M,et al.Identi-fication and quantification of synthetic cannabinoids in‘spicelike’herbal mixtures:A snapshot of the German situation in the autumn of 2012[J].Drug Test Analysis,2014,(6):59-71.
[8]SPADERNA M,ADDY P H,D’SOUZA D C.Spicing things up:synthetic annabinoids[J].Psychopharmacology,2013,228:525-540.
[9]UNODC.World Drug Report[R].New York:United Nations Of-fice on Drugs and Crime,2016.
[10]CHOI H,HEO S,CHOE S,et al.Simultaneous analysis of synthetic cannabinoids in the materials seized during drug traf-ficking using GC-MS[J].Analytical&Bioanalytical Chemis-try.2013,405:3937-3944.
[11]吴中平,郑水庆,严松茂,等.气相色谱-质谱结合准确质量测定快速鉴定合成大麻素[J].分析测试技术与仪器,2012,18(4):197-208.
[12]徐鹏,林文斯,李晓娜,等.UFLC法同时测定新型香料中2个毒品成分的含量[J].药物分析杂志,2013,33(9):1538-1541.
[13]翟晚枫,张春水,高利生.高效液相色谱法同时测定新型香料毒品中的10种合成大麻素[J].分析测试学报,2014,33(8):893-898.
[14]HUTTER M,BROECKER S,KNEISEL S,et al.Identification of the major urinary metabolites in man of seven synthetic can-nabinoids of the aminoalkylindole type present as adulterants in‘herbal mixtures’using LC-MS/MS techniques[J].Journal of Mass Spectrometry.2012,47:54-65.
[15]REID M J,DERRY L,THOMAS K V,et al.Analysis of new classes of recreational drugs in sewage:Synthetic cannabinoids and amphetamine-like substances[J].Drug Test Analysis 2014,(6):72-79.
[16]张春水,翟晚枫.高效液相色谱-三重四极杆质谱法同时测定新型“香料”毒品中的10种合成大麻素[J].分析测试学报,2016,35(3):264-27.
[2]徐鹏,王一,钱振华,等.新型香草香料“毒品”的GC/MS检验1例[J].刑事技术,2011(3):60-61.
[3]梁晨,郑水庆,陈永生,等.检出新型毒品K2一例[J].中国司法鉴定,2011(5):S13-S14.
[4]徐鹏,刘克林,钱振华.首例“Peace Out”香料的GC/MS检验[J].中国药物滥用防治杂志,2012,18(2):120-123.
[5]李茂盛,郑水庆,陈永生,等.GC-MS检测新型策划毒品K3[J].中国司法鉴定,2013,(5):20-23.
[6]EMCDDA.Thematic papers:understanding the“Spice”phe-nomenon[M].Lisbon:European Monitoring Centre for Drugs and Drug Addiction(EMCDDA),2009.
[7]LANGER N,LINDIGKEIT R,SCHIEBEL N M,et al.Identi-fication and quantification of synthetic cannabinoids in‘spicelike’herbal mixtures:A snapshot of the German situation in the autumn of 2012[J].Drug Test Analysis,2014,(6):59-71.
[8]SPADERNA M,ADDY P H,D’SOUZA D C.Spicing things up:synthetic annabinoids[J].Psychopharmacology,2013,228:525-540.
[9]UNODC.World Drug Report[R].New York:United Nations Of-fice on Drugs and Crime,2016.
[10]CHOI H,HEO S,CHOE S,et al.Simultaneous analysis of synthetic cannabinoids in the materials seized during drug traf-ficking using GC-MS[J].Analytical&Bioanalytical Chemis-try.2013,405:3937-3944.
[11]吴中平,郑水庆,严松茂,等.气相色谱-质谱结合准确质量测定快速鉴定合成大麻素[J].分析测试技术与仪器,2012,18(4):197-208.
[12]徐鹏,林文斯,李晓娜,等.UFLC法同时测定新型香料中2个毒品成分的含量[J].药物分析杂志,2013,33(9):1538-1541.
[13]翟晚枫,张春水,高利生.高效液相色谱法同时测定新型香料毒品中的10种合成大麻素[J].分析测试学报,2014,33(8):893-898.
[14]HUTTER M,BROECKER S,KNEISEL S,et al.Identification of the major urinary metabolites in man of seven synthetic can-nabinoids of the aminoalkylindole type present as adulterants in‘herbal mixtures’using LC-MS/MS techniques[J].Journal of Mass Spectrometry.2012,47:54-65.
[15]REID M J,DERRY L,THOMAS K V,et al.Analysis of new classes of recreational drugs in sewage:Synthetic cannabinoids and amphetamine-like substances[J].Drug Test Analysis 2014,(6):72-79.
[16]张春水,翟晚枫.高效液相色谱-三重四极杆质谱法同时测定新型“香料”毒品中的10种合成大麻素[J].分析测试学报,2016,35(3):264-27.