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鸦胆子油中β-谷甾醇的分离与含量测定 被引量:5

Separation and determination of β-sitosterol in Bruceae Fructus oil
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摘要 采用溶剂提取和两次硅胶柱层析法分离鸦胆子油中的β-谷甾醇,并用波谱学方法进行鉴定;对鸦胆子油用氢氧化钾-乙醇皂化后,采用气相色谱法对β-谷甾醇的含量进行测定.色谱条件为AgilentHP5毛细管柱(30m×250μm×0.25μm);FID检测器;进样口温度为285℃;程序升温:270℃ (24min),10℃·min^-1升温至280℃(15min);检测器温度为300℃;分流比为40∶1;流速为1mL·min^-1;进样量为1μL.β-谷甾醇对照品的峰面积与质量浓度在0.02847~0.4100mg·mL^-1呈良好的线性关系(r=0.9994).该方法的平均回收率为95.2%(RSD=2.98%),测得8份样品中β-谷甾醇的质量分数在2.96~4.37mg·g^-1.本方法快速、简便、重复性好,可用于鸦胆子油中β-谷甾醇的含量测定. The β-sitosterol was isolated by solvent extraction and silica gel column chromatography (two times),and identified by spectroscopic methods.A gas chromatography (GC)method was estab-lished for the determination of β-sitosterol in 8 batches of Bruceae Fructus oil.The oil samples of Bruceae Fructus from 8 different areas were analyzed by a Agilent HP-5 capillary column after saponification with KOH-EtOH.The temperature was maintained at 270 ℃ for 24 min,then increased to 280 ℃ at a rate of 10 ℃ ·min -1 and was maintained for 15 min.The injection temperature was 285 ℃ and the detection temperature was 300 ℃.Carrier gas was nitrogen,flow rate was 1.01 mL·min -1 with the spilt 40∶1. The linear range of β-sitosterol was 0.028 47 -0.410 0 mg·mL -1 (r =0.999 4).The average recovery was 95.2% (RSD =2.98%),and the content of β-sitosterol in 8 batches of Bruceae Fructus oil was in the range of 2.96 -4.37 mg·g -1 .The method for determining the content of β-sitosterol was accurate with good reproducibility,and could be used for the determination of β-sitosterol in Bruceae Fructus oil.
出处 《暨南大学学报(自然科学与医学版)》 CAS CSCD 北大核心 2014年第6期519-524,共6页 Journal of Jinan University(Natural Science & Medicine Edition)
基金 广东省自然科学基金团队项目(8351063201000003)
关键词 鸦胆子油 GC Β-谷甾醇 含量测定 Bruceae Fructus oil GC β-sitosterol content determination
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