摘要
目的建立白酒中甜蜜素、三氯蔗糖、阿斯巴甜和纽甜的快速、灵敏、准确的超高效液相色谱-高分辨质谱检测方法。方法样品直接进样,经甲醇-水流动相洗脱,Hypersil GOLD C18(100 mm×2.1 mm,1.8μm)柱分离和Q-Exactive高分辨质谱负离子模式检测,快速获得目标化合物定性、定量信息。结果在质谱分辨率R=70 000、全扫描(fullscan)范围120 m/z^500 m/z检测条件下,4种甜味剂在2μg/L^400μg/L浓度范围内呈现良好的线性关系(r≥0.999);定量限LOQ(S/N=10)分别为1μg/L、0.3μg/L、1μg/L和0.1μg/L。基质加标回收率在97.2%~114.6%之间,相对标准偏差RSD(n=3)≤4%。结论该法具有的高选择性和高灵敏度,避免了样品基质干扰,节省了样品前处理步骤和方法优化环节,能完全满足白酒中痕量甜味剂的快速检测要求。
Objective To establish the rapid,sensitive and accurate detection method of 4 sweeteners（sodium cyclamate,sucralose,aspartame,and neotame） in spirit by ultra performance liquid chromatography-high resolution mass spectrometry（UPLC-HRMS）.Methods Spirit sample was loaded into the column,eluted by methanol-water mobile phase,isolated with column Hypersil GOLD C18（100 mm × 2.1 mm,1.8 μm）,and detected by Q-Exactive high resolution mass spectrometry in negative ion mode,so qualitative and quantitative information was rapidly acquired.Results Under the conditions of full scan mode（120 m/z - 500 m/z） and 70 000 mass resolution,the four sweeteners（Cyclamate,Sucralose,Aspartame and Neotame）had good linear relationship（r≥0.999） with the linear range between 2 μg/L and 400 μg/L.The LOQ（S/N = 10） were1 μg/L,0.3 μg/L,1 μg/L and 0.1 μg/L respectively.The matrix recoveries were between 97.2% and 114.6%.The relative standard deviation RSD（n = 3） were not exceeded 4%.Conclusion High resolution mass spectrum has a high selectivity.It substantially eliminates the sample matrix interference and simplifies the sample preparation.It can fully meet the requirements for rapid detection of sweeteners in spirit.
出处
《中国卫生检验杂志》
北大核心
2014年第22期3244-3246,3250,共4页
Chinese Journal of Health Laboratory Technology
关键词
超高效液相-质谱法
白酒
甜味剂
快速检测
Ultra performance liquid chromatography-high resolution mass spectrometry（UPLC-HRMS）
Spirit
Sweetener
Rapid detection
