超高效液相色谱-串联质谱法同时测定白酒中氨基甲酸乙酯和8种甜味剂

Simultaneous determination of ethyl carbamate and eight sweeteners in Chinese distilled spirit by ultra performance liquid chromatography-tandem mass spectrometry

建立了超高效液相色谱-串联质谱仪（ultra performance liguid chromatograph-tandem mass spectrometry,UPLC-MS/MS）同时测定白酒中氨基甲酸乙酯和8种甜味剂（安赛蜜、糖精钠、甜蜜素、阿斯巴甜、三氯蔗糖、纽甜、阿力甜和甜菊糖苷）含量的新方法。样品经超纯水稀释2倍,微孔滤膜过滤后直接进样,用液相色谱-串联质谱（liguid chromatograph-tandem mass spectrometry,LC-MS/MS）进行定量分析。Waters HSS T3色谱柱为分析柱,甲醇-0.1%乙酸水溶液为流动相进行梯度洗脱,采用电喷雾电离源正负离子切换多反应监测模式检测。结果表明：氨基甲酸乙酯和8种甜味剂在3-500μg/L的范围内线性关系良好（相关系数r〉0.998）,方法检出限在1-3μg/L,基质加标回收率在89%-106%,相对标准偏差≤9%,完全满足日常检测的要求。该方法前处理简单,测定快速、准确、灵敏度高,非常适合白酒中氨基甲酸乙酯和多种甜味剂的快速筛查和定量分析。

An ultra performance liquid chromatography-electrospray ionization tandem mass spectrometric（ UPLC-ESI-MS / MS） method was established for the simultaneous determination of ethyl carbamate and eight sweeteners in Chinese distilled spirit. The samples were diluted with distilled water,and then filtered through 0. 22 μm microporous membrane. The LC separation was performed on a Waters Acquity UPLC system with a HSS T3 column,and0. 1%（ v / v） acetic acid / methanol were used as mobile phase for gradient elution. After LC separation,MS / MS was adopted for multiple reaction monitoring mode（ MRM）. The calibration curves showed good linearity in the range of 3μg / L to 500 μg / L with the correlation coefficients greater than 0. 998. The limits of detection（ LODs） were between1μg / L to 3μg / L. The matrix recoveries were within 89%- 106% and the relative standard deviations（ RSD） were lower than 9%. The results indicated that the proposed method was easier,faster,more sensitive,and suitable for the qualitative and quantitative confirmation of ethyl carbamate and sweeteners in Chinese distilled spirit.