一种高效液相色谱-质谱联用法同时检测凤香型白酒中六种甜味剂的方法

Simultaneous Determination of Six ArtificialSweeteners in Fengxiang Baijiu by High Performance Liquid Chromatography with Mass Spectrometry

建立了一种高效液相色谱三重四级杆质谱联用法同时测定凤香型白酒中的6种人工合成甜味剂(安赛蜜、甜蜜素、糖精钠、阿斯巴甜、三氯蔗糖和纽甜)的分析方法。样品经水浴处理、定容后,过0.22μm滤膜上机分析。以Shin-pack XR-ODSIII C18柱为分离柱,10%甲酸-甲醇为流动相,进行梯度洗脱,经高效液相色谱分离,在ESI负离子模式下扫描,进行多反应监测模式(MRM)检测。结果表明:6种甜味剂的质量浓度与其峰面积在一定范围内线性关系良好,5μg/L^500μg/L范围内相关系数r>0.999,仪器检出限在0.1μg/L^5μg/L之间,方法定量限在0.3μg/L^20.0μg/L之间。6种甜味剂的保留时间和峰面积的相对标准偏差分别在0.565%和4.168%以下,系统精密度良好;样品平均回收率在80.17%~117.90%之间。此方法操作简便,准确可靠,适用于凤香型白酒6种人工合成甜味剂的快速检测。

In this study,we developed a method tosimultaneously detect six artificial weeteners(acesulfame K,saccharinsodium,sodium cyclamate,aspartame,neotame and sucralose)in Fengxiang Baijiu by HPLC-MS/MS.After the sample is treated by water bath and constant volume,and went through 0.22?m filter membrane.Then samples were separated by Shin-pack XR-ODSIII C18 column,using 0.1%formic acid and methanol as mobile phase,gradient elution by high performance liquid chromatography(HPLC)separation,scan in ESI negative ion mode for multiple reaction monitoring mode(MRM)for testing.The results showed that,there was a linear relationship between the mass concentration and the peak area of the six sweeteners:the correlation coefficient r>0.999 in the range of 5~500μg/L,The detection limit of the instrument is between 0.1~5μg/L,and the method limit is between 0.3~20.0μg/L.The relative standard deviations of retention time and peak area of the six sweeteners were below 0.565%and 4.168%,respectively,and the system precision was good,the average recovery of the samples was between 80.17 and 117.90%.The method is simple and quick,accurate and reliable,and is suitable for rapid detection of six artificial sweeteners of Fengxiang Baijiu.