固相萃取/气相色谱-质谱法测定燃香烟气中9种大麻素类新精神活性物质

Determination of Nine Cannabinoids in Incense Smoke by Gas Chromatography-Mass Spectrometry Combined with Solid Phase Extraction-Isotope Dilution

建立了同时测定燃香烟气中9种大麻素类新精神活性物质的气相色谱-质谱(GC-MS)分析方法。样品在燃香烟气收集装置中经溶剂提取,浓缩离心后,采用HLB固相萃取小柱净化,毛细管色谱柱Agilent HP-5MS毛细管柱(30 m×0.25 mm×0.25μm)分离,使用电子轰击电离(EI)源检测,SIM模式进行质谱监测,内标法对9种大麻素类化合物进行定量。结果表明,9种大麻素类化合物在27 min内完成分离分析,并在0.01~4.0 mg/L范围内具有良好的线性关系,相关系数(r^(2))均不小于0.9995,方法的检出限(LOD,S/N=3)和定量下限(LOQ,S/N=10)分别为0.003~0.06 mg/L和0.01~0.2 mg/L。在阴性样品中进行1、2和10倍定量下限的加标回收实验,9种大麻素类化合物的回收率为74.8%~114%,相对标准偏差(RSD,n=6)为1.6%~9.1%。采用该方法对10种市售的燃香样品进行测定,均未检出大麻素类化合物。建立的方法操作简便,可快速对燃香烟气中大麻素类化合物进行定性和定量分析,且能满足发烟量大燃香的检测需求。该方法的建立为我国燃香中大麻素类化合物的监测控制提供了参考。

A comprehensive analytical method based on gas chromatography-mass spectrometry(GC-MS)was developed for the determination of 9 cannabinoid compounds in burnable incense smoke.The smoke of burnable incense sample was extracted with a sampling pump,then enriched into the solvent in a tube.Finally,the solvent was concentrated and centrifuged at 10000 r/min for5 min.The extract was purified on an HLB solid phase extraction column with water containing 10%methyl alcohol as the eluent.The sample was eluted with 6 mL methyl alcohol,and then filtered through a 0.22μm membrane filter unit prior to GC-MS analysis.Temperature-programmed was applied at an initial temperature of 70℃.After 2 min,the temperature was raised to 180℃at a rate of 10℃/min.After 18 min,the temperature was raised to 300℃at a rate of 15℃/min.9 cannabinoid compounds were separated on an Agilent HP-5MS column(30 m×0.25 mm×0.25μm).Identification and quantification were achieved using an electrospray ionization(EI)source under the selected ion monitoring(SIM)mode.The internal standard method was used to quantify the cannabinoids.The results indicated that the 9 compounds could be analyzed within 27 min.The calibration curves showed good linearities for 9 cannabinoid compounds in the range of 0.01-4.0 mg/L,with correlation coefficients(r^(2))not less than 0.9995.The limits of detection(LODs,S/N=3)and limits of quantitation(LOQs,S/N=10)for 9 cannabinoid compounds were in the range of 0.003-0.06mg/L and 0.01-0.2 mg/L,respectively.The average recoveries for 9 cannabinoid compounds were in the range of 74.8%-114%,with relative standard deviations(RSDs,n=6)of 1.6%-9.1%.This method was used to determine 10 types of burnable incense,no new psychoactive substances of cannablis were detected.The method is simple to operate,and could be used for rapid qualitative and quantitative analysis of cannabinoid compounds in burnable incense smoke.