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

Simultaneous Determination of 10 Synthetic Cannabinoids in Novel “Spice”Drugs by HPLC- MS / MS

为测定新型＂香料＂毒品中常见的合成大麻素成分,研究开发了高效液相色谱-三重四极杆质谱联用分析方法。采用安捷伦Poroshell 120 EC-C18（3.0 mm×50 mm,2.7μm）色谱柱,以高纯水-甲醇作流动相进行梯度洗脱,柱温30℃,流速0.3 mL/min。采用电喷雾电离-正离子（ESI＋）、负离子（ESI-）分段检测模式,并对合成大麻素的质谱特征和离子碎裂规律进行研究。结果表明,采用该方法可以实现对常见10种合成大麻素的定性和定量分析,正、负离子模式下检测的目标物分别在1-100,10-1000 ng/mL范围内呈良好线性,日内相对标准偏差（RSD）均不大于3.2%,日间RSD均不大于6.3%。经加标回收率测定和实际样本检验,该方法快速、准确、灵敏、可靠,适用于新型＂香料＂毒品中常见合成大麻素成分的定性定量检测。

Taking into account the high number of synthetic cannabinoids found in seized novel＂spice＂drugs in recent years,this study aimed at the simultaneous determination of common synthetic cannabinoids. An HPLC- MS / MS method was developed for the determination of ten synthetic cannabinoids in novel ＂spice＂drugs. Samples were dissolved with methanol,and then ultrasoundassistedly extracted and filtered through a 0. 22 μm membrane filter. The extract was separated on an Agilent Poroshell 120 EC- C18（ 3. 0 mm × 50 mm,2. 7 μm） column at 30 ℃,using methanol- water as mobile phase. The flow rate was set at 0. 3 mL / min. ESI＋and ESI-mode were used at different times,and the MS spectra characteristics and proposed fragmentation of 10 synthetic cannabinoids were studied. Under the optimized conditions,good linear relationships were obtained in the ranges of 1- 100 ng / mL for 7 synthetic cannabinoids under ESI＋mode,and 10- 1 000 ng / mL for 3 synthetic cannabinoids under ESI-mode. The intra-day relative standard deviations（ RSDs） were not more than 3. 2% and the inter-day RSDs were not more than 6. 3%. This method was applied in real cases,and was proved to be fast,accurate,sensitive and precise for the determination of those 10 common synthetic cannabinoids in novel ＂spice＂drugs.