UPLC-MS/MS同时测定电子烟烟液中安赛蜜等5种合成甜味剂  

Simultaneous determination of 5 synthetic sweeteners in e-liquid by UPLC-MS/MS

作　　者：杨飞[1] 李中皓[1] 严俊[2] 王颖[1] 刘珊珊[1] 邓惠敏[1] 边照阳[1] 范子彦[1] 唐纲岭[1] YANG Fei;LI Zhonghao;YAN Jun;WANG Ying;LIU Shanshan;DENG Huimin;BIAN Zhaoyang;FAN Ziyan;TANG Gangling(China National Tobacco Quality Supervision &Test Center, Zhengzhou 45000,China;China Tobacco Guangxi Industrial Co., Ltd., Nanning 53000,China)

机构地区：[1]国家烟草质量监督检验中心 [2]广西中烟工业有限责任公司,广西南宁北湖南路28号530001

出　　处：《中国烟草学报》2019年第2期1-8,共8页Acta Tabacaria Sinica

摘　　要：【目的】通过对实验条件的优化,建立了一种测定电子烟烟液中5种人工合成甜味剂(安赛蜜、甜蜜素、糖精钠、阿斯巴甜和纽甜)的超高效液相色谱-串联质谱(UPLC-MS/MS)方法。【方法】样品经超纯水稀释、C18分散固相萃取净化后,以BEH C18色谱柱分离,甲醇-0.1%甲酸水溶液为流动相,外标法定量。【结果】结果表明:①5种甜味剂在0.25～5.0μg/mL的标准工作曲线范围内线性关系良好(r>0.998),检出限(LOD)和定量限(LOQ)分别为0.02～0.05和0.07～0.17 mg·kg-1,回收率为92.5%～105.2%,相对标准偏差(RSDs)<5.0%。②采用该方法对10个电子烟烟液样品进行了检测,1个样品检出甜蜜素,含量为2.48 mg·kg-1,2个样品检出纽甜,含量在3.35～4.52 mg·kg-1之间。【结论】该方法操作简单、快速、灵敏度高、有机溶剂消耗少,适用于电子烟烟液中多种甜味剂的同时检测。An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for simultaneous determination of 5 synthetic sweeteners, i.e. Sodium cyclamate, Saccharin sodium, Aspartame, Acesulfame and Neotame, in refill liquids of e-cigarette was developed by optimizing experimental condition. Samples were diluted with ultrapure water and purified by C18. Their extracts were separated on BEH C18 column using methanol-0.1% formic acid as mobile phase. Results were quantified by external standard method. These results showed that: 1) Good linear relation was obtained within the range of standard working solution, with r>0.998. The limits of detection (LODs) and quantification (LOQs) were 0.02~0.05 and 0.07~0.17 mg kg^-1, respectively. The added standard recoveries of blank samples were within the range of 92.5%~105.2%, with a relative standard deviation less than 5.0%. 2) Ten e-cigarette samples were tested by this method. One sample was detected as cyclamate with a content of 2.48 mg kg^-1. Two samples were found to contain neotame, with the content between 3.35 and 4.52 mg kg-1. The method proposed in this study has the advantages of simple operation, rapid speed, high sensitivity and robustness, which is suitable for simultaneous detection of various sweeteners in refill liquids of electronic cigarette.

关 键 词：电子烟 烟液 安赛蜜 甜蜜素 糖精钠 阿斯巴甜 纽甜 UPLC-MS/MS 

分 类 号：O657.63[理学—分析化学] TS458[理学—化学]