超高效液相色谱法同时测定食用植物油中的4种植物甾醇
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(北京市疾病预防控制中心,北京 100013)

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赵海燕 女 高级工程师 研究方向为食品检验 E-mail:yan_zhaohai@sina.com通信作者:┣┣(中)通信作者┫┫赵榕 女 主任技师 研究方向为食品理化 E-mail:Lxyue@yeah.net

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Simultaneous determination of 4 kinds of phytosterols in edible vegetable oil by UPLC
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(Beijing Center for Disease Control and Prevention,Beijing 100013,China)

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    摘要:

    建立超高效液相色谱(UPLC)法测定食用植物油中4种植物甾醇(菜籽甾醇、豆甾醇、菜油甾醇、β-谷甾醇)的方法。方法 食用植物油样品经皂化后,用冰醋酸调节pH=6.0~7.5,乙醇定容后冷冻离心,取上清液测定。采用Endoavorsil C18(100 mm×2.1 mm,1.8 μm)色谱柱,以甲醇作为流动相等度洗脱,使用二极管阵列检测器在波长205 nm下进行检测。结果 方法的线性范围:β-谷甾醇、豆甾醇、菜籽甾醇为20~200 μg/ml;菜油甾醇为10~100 μg/ml,相关系数r均大于0.999 9。方法检出限(S/N=3):菜籽甾醇、豆甾醇、菜油甾醇、β-谷甾醇分别为23.2、18.8、18.6、23.8 μg/g;定量限(S/N=10)分别为77.5、62.8、62.2、79.4 μg/g;4种组分按高、中、低3个浓度水平加标回收率为84.7%~100.7%,相对标准偏差RSD(n=6)均<3%。结论 本方法简便稳定,准确灵敏,适用于食用植物油中4种主要植物甾醇的同时测定。

    Abstract:

    This paper reports an ultra performance liquid chromatography (UPLC) method for determination of 4 kinds of phytosterols (brassicasterol, stigmasterol, campesterol and β-sitosterol) in edible vegetable oil.Methods Edible vegetable oil samples were completely saponificated by glacial acetic acid, pH was adjusted to 6.0-7.5, then used ethanol to constant volume and freezing centrifuged to harvest supernatant. The analytical separation was performed on an Endoavorsil C18 (100 mm×2.1 mm, 1.8 μm) chromatographic column with the isocratic elution using methyl alcohol and detected by photo-diode array detector at 205 nm. Results The linearity ranges were 20-200 μg/ml for β-sitosterol, stigmasterol and brassicasterol and 10-100 μg/ml for campesterol. The limits of detection were 23.2 μg/g for brassicasterol, 18.8 μg/g for stigmasterol, 18.6 μg/g for campesterol, and 23.8 μg/g for β-sitosterol. The quantitation limits were 77.5 μg/g for brassicasterol, 62.8 μg/g for stigmasterol, 62.2 μg/g for campesterol, and 79.4 μg/g for β-sitosterol. The average recoveries of spiked samples were 84.7%-100.7% and the RSD of method (n=6) was less than 3%.Conclusion The method was steady, simple, accurate and sensitive. It could be used to simultaneous detect 4 kinds of phytosterols in edible vegetable oil.

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赵海燕,詹未,李兵,吴国华,赵榕.超高效液相色谱法同时测定食用植物油中的4种植物甾醇[J].中国食品卫生杂志,2016,28(2):223-226.

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  • 收稿日期:2015-12-07
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  • 在线发布日期: 2016-04-20
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