超高效液相色谱-串联质谱法直接测定白酒中8种甜味剂

摘要

建立了超高效液相色谱-串联质谱仪（UPLC-MS/MS）测定白酒中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）含量的分析方法。样品经蒸馏水稀释一定倍数后，过0.22μm微孔滤膜，直接进入UPLC-MS/MS中分析检测。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，在电喷雾电离源负离子模式下，采用多反应监测模式进行检测。结果表明，8种甜味剂在10～500μg/L的范围内线性关系良好（相关系数r＞0.996），方法检出限在1～3μg/L之间，基质加标回收率在89%～106%之间，相对标准偏差≤9%，均可达到白酒中痕量甜味剂的检测要求。该方法前处理简单，测定快速、准确、灵敏度高，非常适合白酒中多种甜味剂的快速筛查和定量分析。%The method of ultra performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) had been developed for simul-taneous determination of eight sweeteners in Baijiu as follows:liquor samples were diluted with distilled water, then filtered through 0.22μm microporous membrane, and LC separation was performed on a Waters Acquity UPLC system with a HSS T3 column, and 0.1%(v/v) acetic ac-id-methanol solution 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 10μg/L to 500μg/L with the correlation coefficients higher than 0.996. The limits of detection (LODs) were between 1μg/L and 3μg/L. The matrix recoveries were within 89%-106%and the relative stan-dard deviations (RSDs) were lower than 9%(n=6). Such method had the advantages including simple pretreatment, fast and accurate measure-ment, and high sensitivity, which was suitable for qualitative and quantitative measurement of sweeteners in Baijiu.