摘要
为建立固相萃取-液相色谱/串联质谱(SPE-HPLC-MS/MS)法同时测定电子烟烟液中安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜、新橙皮甙二氢查尔酮、纽甜、甜菊糖苷等9种甜味剂的方法,以水为萃取溶剂对样品进行超声提取,萃取液经C18硅胶键合固相萃取柱净化和氮吹浓缩,采用Waters XBridge C18色谱柱分离,以甲醇-5 mmol/L乙酸铵的水溶液为流动相进行梯度洗脱,使用电喷雾离子源正负离子切换多反应监测(MRM)模式进行质谱检测,采用华法林钠为内标进行定量。结果表明:①在优化条件下,目标物在各自测试浓度范围内线性良好(R^2均大于0.998),检出限和定量限分别在0.005~0.287μg/mL和0.017~0.956μg/mL之间,加标回收率在82.96%~114.01%之间,RSDs在2.19%~5.18%之间。②对市售8种不同品牌电子烟烟液的检测结果显示,仅在1个样品中检出纽甜,质量分数为5.92 mg/kg。③该方法结果准确可靠,适用于电子烟烟液中9种甜味剂的同时定量检测。
A method coupling solid-phase extraction to high performance liquid chromatography/tandem mass spectrometry(HPLC-MS/MS)was developed to simultaneously determining nine sweeteners(acesulfame,saccharin sodium,sodium cyclamate,sucralose,aspartame,alitame,neohesperidin dihydrochalcone,neotame,and stevioside)in refill liquids for e-cigarettes.The liquid samples were ultrasonically extracted by water,and the extracts were cleaned using SPE column equipped with C18 packing material and concentrated by nitrogen blowing.The analytes were separated on Waters XBridge C18 column using methanol-5 mmol/L ammonium acetate as the mobile phase for gradient elution,determined by tandem mass spectrometry in positive and negative ESI modes under multiple reaction monitoring(MRM),and quantified by using warfarin sodium as internal standard.The results showed that:1)Under the optimal conditions,calibration curves were linear(R^2>0.998)for the nine sweeteners within their test concentration ranges.The limits of detection and quantification were 0.005-0.287μg/mL and 0.017-0.956μg/mL,respectively.The spiked recoveries of blank sample ranged from 82.96%to 114.01%with the relative standard deviations of 2.19%-5.18%.2)The refill liquid samples for eight commercial e-cigarettes of different brands were tested by this method,only one sample was found containing neotame at 5.92 mg/kg.3)This method was accurate,reliable and suitable for the simultaneous determination of nine sweeteners in refill e-liquids.
作者
廖惠云
吴洋
马梦婕
朱怀远
曹毅
陈晶波
张华
朱龙杰
张媛
袁益来
LIAO Huiyun;WU Yang;MA Mengjie;ZHU Huaiyuan;CAO Yi;CHEN Jingbo;ZHANG Hua;ZHU Longjie;ZHANG Yuan;YUAN Yilai(China Tobacco Jiangsu Industrial Co.,Ltd.,Nanjing 210019,China)
出处
《烟草科技》
EI
CAS
CSCD
北大核心
2020年第5期33-40,共8页
Tobacco Science & Technology
基金
江苏中烟工业有限责任公司科技创新项目“细支卷烟用爆珠对逐口烟气中主要香味物质释放量影响研究”(201703),“烟用接装纸中甜味成分质量管控研究”(201911)。
关键词
电子烟
烟液
固相萃取
高效液相色谱-串联质谱
甜味剂
同时测定
E-cigarette
Refill liquid
Solid-phase extraction(SPE)
High performance chromatography/tandem mass spectrometry(HPLC-MS/MS)
Sweetener
Simultaneous determination
