液相串联质谱法测定保健食品中脂溶性维生素方法建立及其应用

Simultaneous Detection of Fat-soluble Vitamins in Health Foods by UPLC-MS/MS and Its Application

目的:建立同时测定保健食品中9种脂溶性维生素的液相色谱-质谱联用法。方法:用适合的有机溶剂充分溶解试样中的脂溶性维生素,超声提取后,采用Waters ACQUITY UPLC BEH C_(18)(100 mm×2.1 mm,1.7μm)色谱柱分离;以0.1%甲酸的甲醇溶液和0.1%甲酸的水溶液为流动相进行梯度洗脱,通过大气压化学电离源多反应监测(MRM)模式进行检测。结果:9种脂溶性维生素在相应的浓度范围内线性关系良好(r≥0.99),方法检出限在0.9~38.3μg/100 g之间。3个添加水平的回收率分别为78.5%~114.9%,RSD为1.57%~11.1%(n=6)。结论:该方法简便、快速、准确、灵敏,适用于营养补充剂类保健食品中脂溶性维生素的测定。

Objective： To develop an ultra-performance liquid chromatography-tandem mass spectrometry （ UPLC - MS/MS ） method for the determination of nine fat-soluble vitamins in health foods. Methods：The samples were extracted by ultrasonic in organic solvents followed by the separation on a Waters ACQUITY UPLC BEH C18 column（100 mm × 2. 1 mm, 1. 7 μm） with gradient elution of 0. 1% formic acid in methanol and 0. 1% formic acid solution as the mobile phase and in a mode of atmosphere pressure chemical i-onization multiple reaction monitoring （MRM）. Results：The method exhibited a good linear relationship （r≥0. 99） with the detection limit between 0. 9 and 38. 3μg/100 g for the nine fat-soluble vitamins. The recoveries were 78. 5%-114. 9% and the RSDs were 1. 57%-11. 1%（n=6）. Conclusion：The analytical method is simple, rapid, accurate and sensitive, and suitable for the determina-tion of fat-soluble vitamins in nutritional supplements.