固相萃取-高效液相色谱-质谱联用法同时测定食品中9种人工合成甜味剂  

Simultaneous determination of nine artificial sweeteners in food by solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry

作　　者：唐吉旺 袁列江[1] 肖泳 王秀 王淑霞 TANG Jiwang;YUAN Liejiang;XIAO Yong;WANG Xiu;WANG Shuxia(Hunan Testing Institute of Product and Commodity Supervison, Changsha 410007, China;The chemical and chemical engineering academy of central south university, Changsha 410083, China)

机构地区：[1]湖南省产商品质量监督检验研究院,湖南长沙410007 [2]中南大学化学化工学院,湖南长沙410083

出　　处：《色谱》2019年第6期619-625,共7页Chinese Journal of Chromatography

基　　金：湖南省质量技术监督局创新驱动计划项目(2017KYJH06)~~

摘　　要：建立了固相萃取-高效液相色谱-串联质谱快速检测食品中安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜、纽甜、甘素及新橙皮甙二氢查尔酮等9种人工合成甜味剂的方法。样品中的甜味剂经三乙胺缓冲溶液(pH4.5)提取,采用亲水亲脂平衡填料固相萃取柱净化,经Phenomenex Knietex■ F5色谱柱(100 mm×2.1 mm, 2.6 μm)分离,以0.1%(v/v)甲酸-5 mmol/L 甲酸铵溶液和甲醇为流动相,进行梯度洗脱,以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。采用内标法定量,进一步降低样品基质效应的影响。结果表明:本方法在去除样品基质干扰方面取得良好效果,9种甜味剂的检出限和定量限分别在2~30 μg/L 和6~100 μg/L 之间,在各自的线性范围内线性关系良好(相关系数 r^2>0.999)。9种甜味剂空白样品在3个水平下的加标回收率在86.3%~106.3%之间,相对标准偏差(RSD)在1.2%~5.9%之间。本方法快捷、高效、准确可靠,可用于复杂食品基质中9种人工合成甜味剂的快速检测。A simple and rapid method based on solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry for the simultaneous determination of nine artificial sweeteners (acesulfame-K, saccharin sodium, cyclamate, sucralose, aspartame, alitame, neotame, dulcin, neohesperidin dihydrochalcone) in various foods was developed. The sweeteners in food samples were extracted with triethylamine buffer solution (pH 4.5) and cleaned using an SPE column equipped with hydrophilic and lipophilic packing material. The analytes were separated on a Phenomenex Knietex■ F5 column (100 mm×2.1 mm, 2.6 μm) using 0.1%(v/v) formic acid-5 mmol/L ammonium formate/methanol as a mobile phase for gradient elution, and then determined by tandem mass spectrometry in positive and negative ESI modes under multiple reaction monitoring (MRM). The internal standard method was used to further suppress the matrix effect. The method proved to be very effective in the removal of matrix interferences. Calibration curves were linear within a studied range of concentrations ( r^2>0.999) for the nine artificial sweeteners. The limits of detection (LODs) and limits of quantification (LOQs) were within 2-30 μg/kg and 6-100 μg/kg , respectively. The recoveries for the nine investigated sweeteners were within 86.3%-106.3% at three spiked levels, with relative standard deviations (RSDs) between 1.2% and 5.9%. The developed method is rapid, efficient, accurate, and reliable;it can also be applied for the rapid determination of other artificial sweeteners in a complex food matrix.

关 键 词：高效液相色谱串联质谱 固相萃取 人工合成甜味剂 食品 

分 类 号：O658[理学—分析化学]