超高效液相色谱法检测固体粉状保健品中豆甾醇、菜油甾醇、β-谷甾醇的含量
目的 建立超高效液相色谱检测固体粉状保健品中豆甾醇、菜油甾醇、β-谷甾醇含量的分析方法。方法 保健品经过KOH和乙醇的皂化反应, 用乙酸调节pH至6.5~7.5, 使用C18色谱柱(100 mm×2. 1 mm, 1.8 μm), 甲醇为流动相, 等梯度洗脱, 用光电二极管阵列检测器在204 nm进行检测。结果 本方法可以在 10 min内完成3种植物甾醇的分离分析。3种植物甾醇线性范围为10~200 mg/L, 线性相关系数均大于0.99。豆甾醇、菜油甾醇、β-谷甾醇的检出限分别为0.095、0.13、0.13 g/100 g (S/N=3), 定量限分别为0.32、0.43、 0.44 g/100 g (S/N=10), 豆甾醇、菜油甾醇、β-谷甾低中高3种浓度的加标平均回收率分别为98.6%~102.9%、96.1%~101.9%和92.3%~98.7%, 6次重复性实验的相对标准偏差(relative standard deviation, RSD)均小于5%。结论 该方法快速、简便、准确、灵敏, 适合测定保健品中豆甾醇、菜油甾醇和β-谷甾醇的含量。
Objective To establish a method for determination of stigmasterol, campesterol and β-sitosterol in solid powder healthy food by ultra performance liquid chromatography Methods Healthy foods were completely saponificated by 50% KOH and ethanol, and the pH was adjusted to 6.0?7.5 by acetic acid. The analytical separation was performed on an C18 chromatographic column (100 mm×2.1 mm, 1.8 μm) with the isocratic elution using methyl alcohol and detected by photo-diode array detector at 204 nm．Results The separation and analysis of 3 plant sterols were completed in 10 min. The linear ranges of 3 plant sterols were 10?200 mg/L and the linear correlation coefficients were all greater than 0.99. The limits of detection of stigmasterol, campesterol and β-sitosterol were 0.095, 0.13 and 0.13 g/100 g (S/N=3), respectively. The limits of quantitative were 0.32, 0.42 and 0.44 g/100 g (S/N=10), respectively. The average recoveries at 3 spiked levels of stigmasterol, campesterol and β-sitosterol ranged from 98.6%-102.9%、96.1%-101.9%和92.3%-98.7%, respectively. The relative standard deviations (n=6) were less than 5%. Conclusion This method is rapid, simple, accurate and sensitive for the determination of stigmasterol, campesterol and β-sitosterol in healthy food.
标题：超高效液相色谱法检测固体粉状保健品中豆甾醇、菜油甾醇、β-谷甾醇的含量
英文标题：Determination of stigmasterol, campesterol and β-sitosterol in solid powder healthy food by ultra performance liquid chromatography
作者：
杜茹芸 上海市质量监督检验技术研究院
徐红斌 上海市质量监督检验技术研究院
周耀斌 上海市质量监督检验技术研究院
中文关键词:保健品,豆甾醇,菜油甾醇,β-谷甾醇,超高效液相色谱法,
英文关键词:healthy food,stigmasterol,campesterol,β-sitosterol,ultra-high performance liquid chromatography,
发表日期：2019-08-06
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