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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 a rapid, sensitive and accurate ultra-high performance liquid chromatography-high resolution mass spectrometry method for determination of sodium cyclamate, sucralose, aspartame and neotame in liquor. Methods The samples were directly injected into the column and eluted with methanol-water mobile phase. The column was separated on a Hypersil GOLD C18 (100 mm × 2.1 mm, 1.8 μm) column and detected by Q-Exactive high resolution mass spectrometry negative ion mode to obtain qualitative and quantitative information of the target compound. Results The results showed that there was a good linear relationship between the concentration of 4 kinds of sweeteners in the range of 2μg / L to 400μg / L under the conditions of mass spectral resolution R = 70 000 and full scan range 120 m / z ~ 500 m / (r≥0.999), LOQ (S / N = 10) were 1μg / L, 0.3μg / L, 1μg / L and 0.1μg / L, respectively. The recoveries of matrix spiked were between 97.2% and 114.6%, and the relative standard deviations RSD (n = 3) ≤4%. Conclusion The method has high selectivity and high sensitivity, avoids sample matrix interference, saves sample pretreatment steps and method optimization steps, and can fully meet the rapid detection requirements of trace amounts of sweeteners in white spirit.