气相色谱-串联质谱法测定电子烟烟液中的10种生物碱含量  

Determination of 10 Alkaloids in Refill Solutions for Electronic Cigarettes by Gas Chromatography-Tandem Mass Spectrometry

作　　者：严俊[1] 王红娟[2] 陈志燕[1] 陈欢[2] 周芸[1] 罗彦波[2] 范忠[1] 付亚宁[2] 邓宾玲[1] 刘彤[2] 韦入丹 黄世杰[1] 韩书磊[2] YAN Jun;WANG Hong-juan;CHEN Zhi-yan;CHEN Huan;ZHOU Yun;LUO Yan-bo;FAN Zhong;FU Ya-ning;DENG Bin-ling;LIU Tong;WEI Ru-dan;HUANG Shi-jie;HAN Shu-lei(China Tobacco Guangxi Industrial Co.,Ltd.,Nanning 530001,China;China National Tobacco Quality Supervision and Test Center,Zhengzhou 450001,China)

机构地区：[1]广西中烟工业有限责任公司,广西南宁530001 [2]国家烟草质量监督检验中心,河南郑州450001

出　　处：《分析测试学报》2021年第7期1037-1042,共6页Journal of Instrumental Analysis

基　　金：中国烟草总公司科技重大专项项目(110202001006(XX-02),110202001007(XX-03));国家烟草质量监督检验中心科技创新项目(552017CA0030);广西中烟工业有限责任公司科技计划项目(GXZYCX2019C006)。

摘　　要：建立了一种气相色谱-串联质谱法测定电子烟烟液中10种生物碱含量的分析方法,并对仪器分析条件、样品前处理条件等进行了优化。样品加入2.0 mL 2%NaOH水溶液后,以10 mL二氯甲烷-甲醇溶液(体积比4∶1)为萃取溶液,涡旋振荡萃取30 min,萃取液经无水硫酸镁除水后,以气相色谱-串联质谱法多反应监测(MRM)模式检测。结果显示:在优化条件下,烟碱及9种次要生物碱在25~1000μg/mL及0.0025~20μg/mL范围内呈良好的线性,相关系数(r^(2))不低于0.997,3个加标水平下的回收率为87.9%~109%,日内及日间精密度(RSD)分别不高于6.8%和7.9%,检出限(LOD)为0.0040~0.10 mg/kg,定量下限(LOQ)为0.013~0.33 mg/kg。用该方法测定23种品牌共计171种型号电子烟烟液中10种生物碱含量,结果发现,电子烟烟液中的烟碱含量为2.16~23.73 mg/g,9种次要生物碱的含量中位值为0.06~7.35 mg/kg,检出率为64.91%~99.42%,其中9种电子烟烟液样品的总次要生物碱含量与烟碱含量比例大于1.0%。该方法灵敏度高、准确性好、重复性好,完全满足电子烟烟液样品中10种生物碱的检测要求。A gas chromatography-tandem mass spectrometry(GC-MS/MS)method was established for the simultaneous determination of 10 alkaloids in refill solutions for electronic cigarettes.The instruments and pretreatment conditions were critically examined.The sample was added with 2.0 mL of 2%sodium hydroxide and extracted for 30 min with 10 mL of dichloromethane/methyl alcohol(4∶1,by volume).The sample extracts were determined by gas chromatography-tandem mass spectrometry under multiple reaction monitoring(MRM)mode after removal of water with anhydrous magnesium sulfate.Results showed that nicotine and nine minor alkaloids presented good linear relationships in the concentration range of 25-1000μg/mL and 0.0025-20μg/mL,respectively.The linear correlation coefficients were above 0.997,the limits of detection(LOD)ranged from 0.0040 mg/kg to 0.10 mg/kg,the limits of quantitation were 0.013-0.33 mg/kg,the recoveries ranged from 87.9%to 109%at three spiked levels,and the relative standard deviations(RSDs)for both intra-and inter-day were no more than 6.8%and 7.9%,respectively.The results indicated that the method was sensitive,accurate and reproducible,and suitable for the determination of 10 alkaloids in refill solutions for electronic cigarettes.The method was successfully applied to the analysis of 171 refill solutions for 23 brands.Nicotine levels in refill solutions varied considerably,ranging from 2.16 mg/g to 23.73 mg/g.The median concentrations of nine minor alkaloids were 0.06-7.35 mg/kg,with the detection rate ranging from 64.91%to 99.42%.The proportion of total minor alkaloids to nicotine content in nine electronic cigarette liquid samples was more than 1.0%.

关 键 词：生物碱 液液萃取 气相色谱-串联质谱 电子烟烟液 

分 类 号：O657.7[理学—分析化学]