摘要
建立了一种同时检测白酒中最常见的7种人工合成甜味剂(安赛蜜、糖精钠、甜蜜素、纽甜、三氯蔗糖、阿斯巴甜、甜菊糖苷)的超高效液相色谱-串联质谱(UPLC-TQS)检测方法。白酒样品于120℃电热板加热去酒精处理后,用超纯水定容,过0.22μm滤膜后进行UPLC-TQS分析。样品以甲醇和0.1%甲酸水作为流动相梯度洗脱,经ACQUITY UPLC HSS T3(100 mm×2.1 mm, 1.8μm)色谱柱,流速为0.35 mL/min,柱温为40℃,采用电喷雾电离源负离子模式检测,进样时间为6.5 min。经检测,7种甜味剂在各自的线性范围内均有较好的线性关系,线性相关系数R2均大于0.999。检出限在0.1～6 ng/mL。加标回收率为91.8%～114%。该方法简单、快速,结果准确,灵敏度高,可直接用于白酒中7种甜味剂的日常监督检测。
In this study, a method for simultaneous detection of seven most commonly-used synthetic sweeteners (acesulfame, sodium saccharin, sodium cyclamate, neotame, sucralose, aspartame, and stevioside) in Baijiu by ultra performance liquid chromatographytandem mass spectrometry (UPLC-TQS) had been developed as follows: Baijiu samples heated to 120 ℃ on hot plate to remove the alcohol, made up to constant volume with ultrapure water, then filtered by 0.22 μm filter, and finally analyzed by UPLC-TQS. The samples were gradient-eluted with methanol and 0.1 % formic acid as the mobile phase on ACQUITY UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm) with a flow rate of 0.35 mL/min and a column temperature at 40 ℃ by using electrospray ionization source in negative ion mode with the injection time as 6.5 min. All the seven sweeteners had a good linear relationship in their individual linear ranges, and the linear correlation coefficient R^2 was above 0.999. The detection limit was between 0.1 ng/mL to 6 ng/mL. The spiked recoveries were 91.8 % to 114 %. The method was simple, rapid, accurate, and sensitive, and it could be directly used for daily monitoring and detection of seven sweeteners in Baijiu.
作者
白丽真
刘伟
刘洪银
张帆
BAI Lizhen;LIU Wei;LIU Hongyin;ZHANG Fan(Niulanshan Distillery,Beijing 101301,China)
出处
《酿酒科技》
2019年第4期108-112,共5页
Liquor-Making Science & Technology
