在线固相萃取/液相色谱-串联质谱法测定水中合成大麻素及代谢物  

Determination of Synthetic Cannabinoids and Metabolites in Water by On-line Solid Phase Extraction/Liquid Chromatography-Tandem Mass Spectrometry

作　　者：蒋力维 杨哲 吴一荻 杨思瑶 李佳益 吕建霞 JIANG Li-wei;YANG Zhe;WU Yi-di;YANG Si-yao;LI Jia-yi;LÜJian-xia(National Narcotics Laboratory Beijing Regional Center,Beijing 100164,China;School of Criminal Investigation,People’s Public Security University of China,Beijing 100038,China)

机构地区：[1]国家毒品实验室北京分中心,北京100164 [2]中国人民公安大学侦查学院,北京100038

出　　处：《分析测试学报》2024年第12期1873-1882,共10页Journal of Instrumental Analysis

基　　金：北京市科技计划资助项目(Z221100005222006)。

摘　　要：建立了在线固相萃取/液相色谱-串联质谱(on-line SPE/LC-MS/MS)同时测定水中71种合成大麻素和16种代谢物的分析方法。取40 mL水样配制成20%的甲醇水溶液,加入乙酸铵与内标物后采用聚四氟乙烯(PTFE)滤膜过膜。取1500μL过滤样,经亲水-疏水平衡(HLB)固相萃取柱(30 mm×2.1 mm,20μm)净化和富集,采用C_(18)色谱柱(100 mm×2.1 mm,1.9μm),以1 mmol/L甲酸铵水溶液和甲醇-乙腈(体积比1∶1)为流动相进行洗脱分离,电喷雾电离源正离子方式和多反应监测(MRM)模式检测,内标法定量。结果表明,87种目标物在1~200 ng/L范围内线性关系良好,相关系数均大于0.990,定量下限为0.03~0.73 ng/L。以自来水、地表水和生活污水为基质,在2、75、150 ng/L加标水平下,除N-(1-氨甲酰基-2,2-二甲基丙基)-吲唑-3-甲酰胺和N-(1-氨基-3,3-二甲基-1-氧代丁-2-基)-1-(4-丁酸)-1H-吲唑-3-甲酰胺2种物质外,其余85种目标物的加标回收率为60.4%~130%,相对标准偏差(RSD,n=6)为0.20%~9.8%。该方法简单、快速,能满足水样中85种痕量合成大麻素类物质的分析要求。In this study,an analytical method was established for simultaneous determination of 71 synthetic cannabinoids and 16 metabolites in water by on-line solid phase extraction/liquid chromatography-tandem mass spectrometry(on-line SPE/LC-MS/MS).Through the optimization of instrument analysis and sample preparation,the best experimental conditions were obtained.10 mL methanol was added into 40 mL water to prepare a solution containing 20%(by volume) methanol.After adding ammonium acetate and internal standards,the solution was filtered through a PTFE filter.1 500 μL of the filtered solution was injected into the HLB SPE columns(30 mm×2.1 mm,20 μm) for purification and enrichment.The analytes were separated by using a C_(18) chromatographic column(100 mm×2.1 mm,1.9 μm),with 1 mmol/L ammonium formate aqueous solution and methanol-acetonitrile(1∶1) as the mobile phase for elution.The detection was carried out with electrospray ion source in positive ion mode under multiple reaction monitoring mode(MRM),and quantified with internal standard method.The results showed that in the linear range of 1-200 ng/L,the linear correlation coefficients of 87 target analytes were all greater than 0.990,and the limits of quantification were 0.03-0.73 ng/L.Except of SC-0862 and ADB-BUTINACA N-butanoic acid metabolite,the recoveries of 85 target analytes ranged from 60.4% to 130% at the three spiked levels of 2,75,150 ng/L,while the relative standard deviations(RSDs,n=6) were between 0.20% and 9.8% in tap water,surface water and waste water.The method is simple,rapid,and could meet the requirements for the quantitative analysis of 85 synthetic cannabinoids and related metabolites in water samples.

关 键 词：在线固相萃取/液相色谱-串联质谱法 水 合成大麻素 代谢物 

分 类 号：O657.63[理学—分析化学] O657.7[理学—化学]