高效液相色谱-质谱法测定酒中甜蜜素含量的研究

Determination of sodium cyclamate in wine by UPLC-MS/MS

目的本文采用UPLC-MS/MS法对市售30种酒中甜蜜素进行测定。方法采用Acquity UPLCTM BEH C18(2.1 mm×100 mm,1.7μm)色谱柱分离,甲醇-0.1%乙酸(90+10)作为流动相洗脱,运用三重四极杆质量分析器定性定量分析。结果该方法测定酒中甜蜜素具有良好的线性关系,测定方法检出限为0.010μg/ml,定量限为0.021μg/ml,加标回收率为75.0%～105%,精密度RSD值为10.5%～12.1%。30种酒样品中,有13个样品检测出甜蜜素,含量水平为0.027～891μg/ml。结论该方法测定酒中甜蜜素,具有较高的灵敏度和选择性,样品测定结果表明存在乱用甜蜜素现象。

Objective A comprehensive analytical method based on UPLC-MS/MS was established for determination of sodium cyclamate in 30 wine samples from markets. Methods UPLC separation was performed on an Acquity UPLCTM BEH Cls column （2. 1 mm×100 mm, 1.7 μm） with methanol-0.1% acetic acid （90±10） as mobile phase. Triple- quadrupole mass spectrometry analyzer was used for the qualitative and quantitative analysis. Results The limit of detection of sodium cyclamate was 10 μg/L. The recoveries of Sodium cyclamate were 75.0% - 105% , and the RSD was 10. 5% - 12.1%. Among 30 wine samples, 13 samples were found to contain sodium cyclamate, whose level was 0. 027 - 891μg/ml. Conclusion The method is simple with high sensitivity and selectivity and suitable for the determination of sodium cyclamate in wine. The results indicated the presence of abuse of sodium cyclamate.