HPLC-MS/MS法快速测定电子烟油中58种合成大麻素

58 Synthetic Cannabinoids Rapidly Determined from Electronic Cigarette Oil by HPLC-MS/MS

本文旨在建立一套高效液相色谱-串联质谱法(HPLC-MS/MS)快速定性定量检测电子烟油中58种合成大麻素的分析方法。在研究中,选择适宜液相色谱柱,对色谱条件和质谱条件进行优化。样品中的目标物经甲醇萃取后,使用五氟苯基丙基(PFPP)色谱柱(100 mm×2.1 mm×5μm)分离,以乙腈和20 mmol/L乙酸铵+0.1%(体积分数)甲酸缓冲水溶液为流动相进行梯度洗脱,在电喷雾离子源正离子(ESI+)模式下,采用动态多反应监测模式(d-MRM)测定,使用特征离子碎片的峰面积进行外标法定量。结果表明,58种合成大麻素在0.5~50 ng/mL浓度范围内线性关系良好,R2均大于0.99;检出限(LOD,S/N=3)为0.5~1μg/g,定量限(LOQ,S/N=10)均为2μg/g;58种合成大麻素在空白基质中高、中和低三个添加水平下的平均回收率为89.9%~144.0%,相对标准偏差均小于15%;基质效应考察结果表明,78%的合成大麻素呈现为基质增强效应,其他为基质抑制效应;仅5%的合成大麻素表现为强基质效应,其他为中等或弱基质效应;采用基质匹配标准曲线校正,可有效降低基质效应的影响。将该方法应用于本年度内深圳市办案机关提供的电子烟油检测,其中涉及的6种合成大麻素均被准确筛查和定量检测。该方法操作简单,检测覆盖范围广,耗时少,准确度高且检出限低,适用于电子烟油中合成大麻素的快速筛查和定量分析。

Synthetic cannabinoids(SCs),among the most abused new psychoactive substances,own a structure similar to tetrahydrocannabinol and ability to activate cannabinoid receptors,therewith capable of triggering more intense excitatory and hallucinogenic effects.SCs are mainly detected for identifi cation of drug-related criminal cases about those evidential materials from plant,hair,blood,urine and other biolgoical stuffs.Presently,electronic cigarette oil has sometimes been found of illicit addition of SCs,leaving it into requirement of forensic identifi cation.Liquid chromatography-mass spectrometry(LC-MS)is used most widely for SCs to be separated and detected.Here,a method was established for rapid qualitative and quantitative determination of 58 synthetic cannabinoids from electronic cigarette oil by high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).The suitable liquid chromatographic column was selected to optimize the chromatographic and mass spectrometric conditions.The electronic cigarette oil,spiked of 58 SCs standards,was extracted with methanol and then undergone into separation by pentafl uorophenylpropyl(PFPP)column(100 mm×2.1 mm×5μm)through the buffered solution of gradient-eluting acetonitrile and 20 mmol/L ammonium acetate plus 0.1%(V/V)formic acid.Under the electrospray positive ion sourcing(ESI+)mode,the dynamic multiple reaction monitoring mode(d-MRM)was adopted to determine the peak area of characteristic ion fragments from the external standards.The experimental results showed that the 58 synthetic cannabinoids were of good linear relationship in the concentration range of 0.5~50 ng/mL,having R2 greater than 0.99,detection limit(LOD,S/N=3)and quantitative limit(LOQ,S/N=10)as the respective 0.5~1μg/g and 2μg/g,together with the average recoveries as 89.9%~144.0%and relative standard deviation less than 15%.Matrix effect turned out 78%of the tested synthetic cannabinoids being enhanced and the others inhibited.Alternately,only 5%of the tested synthetic cannabinoids were of strong matrix effect and the others of medium or weak.Fortunately,matrix-matching standard curve correction had effectively reduced the infl uence of matrix effect.The established method was also applied into detecting the electronic cigarette oils provided from actual cases,having the involved six synthetic cannabinoids accurately screened and quantitatively detected.Therefore,an expectation could be put on the method to use for rapid determination of synthetic cannabinoids illicitly added into electronic cigarette oil with its merits of simple operation,wide detection coverage,less timeconsuming,high accuracy and low detection limit.