固相萃取—GC/MS法测定油脂胆固醇含量的研究

摘要

建立了固相萃取- GC/MS法测定油脂中胆固醇含量的分析方法,用氟罗里硅土小柱提取和纯化油脂样品中的待测化合物后,GC/MS用HP -5毛细管柱分离,以选择离子模式(SIM)进行定性定 量分析.在0.1 ～ 25mg/L的浓度范围内浓度与峰面积具有良好的线性关系,相关系数(r)为0.9994,在1、5、20mg/kg三个加标水平下进行方法验证,平均回收率为86.1％～103.0％之间,相对标准偏差为1.82％ ～ 5.47％,方法检出限为0.11 mg/kg.该法操作简单,准确度高,重现性好,是目前测定油脂中胆 固醇含量较为理想的方法.%A solid phase extraction(SPE)-CC/MS method was developed to indentify the batch of Cholesterol in fat, which is derived by using heptaflurobutyrylimidazole (HFBI) and then separated, identified and quantified by Gas Chromatograph-Mass employing HP-5 capillary column in SIM mode. The linearity of this method was ranged from 0. Lmg/L to 25mg/L. The method was validated at the spike levels of 1,5 ,20mg/kg. The validation results indicated that the average recoveries of cholesterol ranged from 86.1% - 103. 0% with a relative standard deviation of 1. 82% -5. 47%. This method was sensitive, accurate, precise and simple for batch of cholesterol.