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作 者:辜英杰[1] 吴锐[1] 闫世平[1] 牟德海[1] 苏流坤[1] 农云军[1] 郑家概[1]
机构地区:[1]中国广州分析测试中心广东省化学危害应急检测技术重点实验室,广东广州510070
出 处:《分析测试学报》2006年第6期98-100,共3页Journal of Instrumental Analysis
摘 要:建立了可满足各类食品(包括动物性食品、动植物混合食品)中胆固醇的HPLC—ELSD快速测定方法。样品经50%(w)KQH直接皂化和石油醚萃取后进行色谱分析。色i普柱为ODS柱,流动相为乙醇和乙脯,通过优化梯度洗脱条件,在20min内实现了胆固醇与干扰物质(如植物甾醇)的有效分离,分离度月大于1.5。胆固醇色谱峰面积的自然对数与浓度的自然对数呈良好的线性关系(r〉0.9996),检出限(LOD)为0.20μg(S/N=3),定量下限(LOQ)为0.56μg(S/N=10),回收率为93%-96%(n=6),重复性RSD〈3.0%(n=6)。A simple, rapid and accurate method was developed for determination of cholesterol in a variety of foods, including animal and plant originated foods, by high performance liquid chromatography (HPLC) with evaporative light -scatter detector (ELSD). After directly saponified with 50% (w) KOH, the sample was extracted with petroleum ether. The extract was then separated on an ODS column and eluted by mobile phases consisted of ethanol and acetonitrile with a gradient program. Cholesterol was separated satisfactorily with interferences such as phytosterols in 20 minutes with R 〉 1.5. The logarithm of peak areas of cholesterol was plotted against the logarithm of the concentration of standard solutions, and a linear regression coefficient of 0. 999 6 was obtained in the range of 20 - 1 200 mg/L. Limit of detection(LOD) was 0. 20 μg( S/N = 3 ) and limit of quantification(LOQ) was 0.56 μg( S/N =10). Recoveries of 93%- 96% (n = 6) were obtained by spiking experiments. The repeatability ( RSD, n = 6) of the method was less than 3.0%.
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