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目的在胆固醇的HPLC测定GB/T 22220—2008方法的基础上进行改进,新建一种快速、准确的检测食品中胆固醇的超高效液相色谱方法。方法样品在60℃恒温振荡器中皂化,提取,用冰醋酸调节p H值,乙醇定容,UPLC定量分析。采用DIKMA Endeavorsil C18色谱柱(50 mm×2.1 mm,1.8μm),甲醇为流动相,PDA检测器在波长205 nm下进行检测。结果胆固醇在10.0μg/ml~300μg/ml时,线性关系良好,相关系数(r)>0.999 9,检出限为35.4μg/g。猪肉样品在3种添加水平下,胆固醇的平均回收率分别为107.8%、101.8%、103.0%,加蛋黄样品在3种添加水平下,胆固醇的平均回收率分别为101.7%、101.8%、102.4%。猪肉样品和鸡蛋黄样品中胆固醇的相对标准偏差(RSD)分别为3.25%、3.47%。结论将本方法和GB/T 22220—2008方法同时应用在肉和蛋的胆固醇检测中,本方法更简便、快速、准确、重现性好,适用于食品中胆固醇含量的测定。
OBJECTIVE To improve on the basis of HPLC determination of cholesterol GB / T 22220-2008 and to establish a fast and accurate ultra-high performance liquid chromatography method for the determination of cholesterol in food. Methods The samples were saponified in a constant temperature shaker at 60 ° C and extracted. The pH value was adjusted with glacial acetic acid, and the volume of ethanol was determined by UPLC. A DIKMA Endeavorsil C18 column (50 mm × 2.1 mm, 1.8 μm) was used with methanol as the mobile phase and the PDA detector at 205 nm. Results Cholesterol had a good linearity at a concentration of 10.0μg / ml ~ 300μg / ml with a correlation coefficient (r)> 0.999 9 and a detection limit of 35.4μg / g. The average recoveries of cholesterol in the pork samples were 107.8%, 101.8% and 103.0% at the three addition levels, respectively. The average recoveries of cholesterol at the three addition levels were 101.7%, 101.8% and 102.4% . The relative standard deviations (RSDs) of cholesterol in pork samples and egg yolk samples were 3.25% and 3.47%, respectively. Conclusion The method and GB / T 22220-2008 method applied to the simultaneous detection of cholesterol in meat and eggs, the method is simple, rapid, accurate and reproducible, and is suitable for the determination of cholesterol content in food.