RS-GC-MS/MS法测定乳源性保健品中维生素E和胆固醇

Determination of vitamin E and cholesterol in milk derived health products by RS-GC-MS/MS

本文建立了一种快速皂化萃取-气相色谱-串联质谱法测定乳源性保健品中4种生育酚和胆固醇的方法。样品经脂肪酶酶解4h后,采用碳酸钾-乙醇快速法皂化,在35℃下条件下皂化10min,由正己烷萃取20min后,经HP-5MS色谱柱分离,在GC-MS/MS多反应监测离子模式下进行定性和定量分析。结果表明,4种生育酚和胆固醇在0.5~50.0μg/mL浓度范围内线性良好,相关系数R为0.9992~0.9997,检出限范围为0.01~0.20mg/kg,定量限范围为0.03~0.60mg/kg。三个水平的加标回收率范围为88.2%~97.1%,相对标准偏差(RSD)为2.3%~5.8%,可以满足乳源性保健品中4种生育酚和胆固醇定性和定量检测的需求。

A method for the determination of four kinds of tocopherols and cholesterol in milk derived health products by gas chromatography-tandem mass spectrometry with rapid saponification and extraction was established.The samples were enzymolyzed by lipase for 4h,then saponified at 35℃for 10min by potassium carbonate ethanol,finally extracted with n-hexane for 20min,separated by HP-5 MS column,and analyzed by GC-MS/MS multi reaction monitoring ion mode scanning.The results showed that the linearity of four kinds of tocopherols and cholesterol in the concentration range of 0.5~50.0μg/mL was good.The correlation coefficient R was 0.9992~0.9997.The detection limit was 0.01~0.20mg/kg.The quantitative limit was 0.03~0.60mg/kg.The recoveries of the three levels were 88.2%~97.1%,and the RSD was 2.3%~5.8%.It can meet the requirements of qualitative and quantitative detection of the four kinds of tocopherols and cholesterol in milk derived health products.