LC-MS/MS Determination of 6 Synthetic Cannabinoids in Plant Sample
摘 要
采用液相色谱-串联质谱法测定植物样品中6种合成大麻素的含量。植物样品20 mg经甲醇50 mL超声提取30 min,离心后取上清液,以C18色谱柱为分离柱,以不同体积比的甲醇和水混合液为流动相进行梯度洗脱,采用电喷雾正离子源多反应监测模式检测。6种合成大麻素的质量浓度均在一定范围内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.2~3.0 μg·L-1。加标回收率为95.9%~104%,测定值的日内相对标准偏差(n=5)均小于6.5%,日间相对标准偏差(n=5)均小于8.0%。
Abstract
LC-MS/MS was applied to the determination of 6 synthetic cannabinoids in plant sample. The plant sample (20 mg) was extracted ultrasonically with 50 mL of methanol for 30 min. After centrifugation, the supernatant obtained were used for LC-MS/MS determination. C18 chromatographic column was used as stationary phase, and the mixture of methanol and water mixed in different ratios was used as mobile phase in gradient elution. ESI+ and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 6 synthetic cannabinoids were kept in definite ranges, with detection limits (3S/N) in the range of 0.2-3.0 μg·L-1. Values of recovery found by standard addition method were in the range of 95.9%-104%, values of intra-day RSD's (n=5) less than 6.5% and inter-day RSD's (n=5) less than 8.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201711010
所属栏目 工作简报
基金项目 辽宁省教育厅科学研究一般项目(L2014510)
收稿日期 2016/11/20
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备注徐秀明(1980-),女,山东淄博人,讲师,博士,主要从事毒品毒物的教学与科研工作,xuxm80@163.com
引用该论文: XU Xiuming. LC-MS/MS Determination of 6 Synthetic Cannabinoids in Plant Sample[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(11): 1291~1295
徐秀明. 液相色谱-串联质谱法测定植物样品中6种合成大麻素[J]. 理化检验-化学分册, 2017, 53(11): 1291~1295
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参考文献
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【2】WOHLFARTH A, SCHEIDWEILER K B, CHEN X H, et al. Qualitative confirmation of 9 synthetic cannabinoids and 20 metabolites in human urine using LC-MS/MS and library search[J]. Anal Chem, 2013,85:3730-3738.
【3】SEBASTIAN D, STEFAN K, WOLFGANG W, et al. Development and validation of a liquid chromatography-tandem mass spectrometry method for the quartitation of synthetic cannabinoids of the aminoalkylindole type and methanandamide in serum and its application to forensic samples[J]. J Mass Spectrom, 2011,46:163-171.
【4】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.
【5】徐鹏,李晓娜,刘克林,等.UFLC法测定新型"spike99"香料中JWH-073的含量[J].中国法医学杂志, 2012,27(6):477-479.
【6】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):120-122.
【7】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.
【8】CHOI H, HEO S, CHOE S, et al. Simultaneous analysis of synthetic cannabinoids in the materials seized during drug trafficking using GC-MS[J]. Anal Bioanal Chem, 2013,405:3937-3944.
【9】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.
【10】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.
【11】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.
【12】HUTTER M, BROECKER S, KNEISEL S, et al. Identification of the major urinary metabolites in man of seven synthetic cannabinoids of the aminoalkylindole type present as adulterants in ‘herbal mixtures’ using LC-MS/MS techniques[J]. J Mass Spectrom, 2012,47:54-65.
【13】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.
【14】KNEISEL S, AUWARTER V. Analysis of 30 synthetic cannabinoids in serum by liquid chromatography-electrospray ionization tandem mass spectrometry after liquid-liquid extraction[J]. J Mass Spectrom, 2012,47:825-835.
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