摘要
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,1.8μm),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.
作者
杜茹芸
徐红斌
周耀斌
DU Ru-Yun;XU Hong-Bin;Zhou Yao-Bin(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 200233,China)
出处
《食品安全质量检测学报》
CAS
2019年第21期7189-7193,共5页
Journal of Food Safety and Quality
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
healthy food
stigmasterol
campesterol
β-sitosterol
ultra-high performance liquid chromatography