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中国药物评价 ›› 2024, Vol. 41 ›› Issue (6): 464-469.

• 评价技术与方法 • 上一篇    下一篇

药用辅料大豆油、橄榄油中甾醇组分的检测及分析

李沫, 黄海, 徐万魁*   

  1. 辽宁省药品检验检测院, 国家药品监督管理局化学药品质量研究与评价重点实验室,
         辽宁 沈阳 110036
  • 收稿日期:2023-12-11 出版日期:2024-12-28 发布日期:2024-12-28
  • 基金资助:
    辽宁省自然基金资助计划“基于脂肪乳类制剂安全风险控制的油脂类辅料质量控制研究”项目(编号:2022-MS-096)

Determination and Analysis of Sterols in Pharmaceutical Lipid Excipients Soybean Oil and Olive Oil

  1. Liaoning Institute for Drug Control, Liaoning Shenyang 110036, China
  • Received:2023-12-11 Online:2024-12-28 Published:2024-12-28

摘要: 目的:建立油脂类辅料大豆油及橄榄油中甾醇的检测方法,并对其甾醇组成进行分析。方法:从油脂类辅料中提取出不皂化物,再用HPLC法从不皂化物中分离并收集甾醇组分,采用的色谱柱为Kromasil 60-5SIL硅胶柱(250 mm×4.6 mm,5 μm)及同填料的预柱(5 mm×4.6 mm,5 μm),流动相为正己烷-异丙醇(99∶1),检测波长为210 nm,流速为1 mL·min-1。收集到的馏分经过衍生化处理后,采用GC法进行分离分析,采用固定液为5%苯基-95%甲基聚硅氧烷的毛细管色谱柱,进样口的温度:290 ℃,检测器的温度:290 ℃,升温程序:起始柱温270 ℃,维持50 min,以5 ℃·min-1的速率升温至290 ℃,维持25 min;载气为氦气。结果:大豆油中甾醇组分由高到低依次为:β-谷甾醇、菜油甾醇、豆甾醇,3种甾醇组分占甾醇总数的85%以上;橄榄油中甾醇组分由高到低依次为:β-谷甾醇、菜油甾醇、谷甾烷醇,3种甾醇组分占甾醇总数的93%。结论:该方法可用于油脂类辅料中甾醇组成的检测,不同类型的油脂甾醇组成和占比不同,可进一步研究建立油脂类辅料的甾醇指纹图谱,用于油脂的鉴别、掺假的判定。

关键词: font-size:medium, "> , 油脂类辅料;大豆油;橄榄油;甾醇组成

Abstract: Objective: To establish a detection method for sterol in soybean oil and olive oil, and analyze the sterol composition. Methods:Extract unsaponifiable matter from oil excipients, then use the HPLC method to separate and collect sterol components from the unsaponifiable matter, the chromatographic column was Kromasil 60-5SIL silica gel column(250 mm×4.6 mm, 5 μm)and pre-column (5 mm×4.6 mm, 5 μm)with the same packing, use n-hexane-isopropanol (99∶1) as the mobile phase, 210 nm as the detection wavelength, and the flow rate was 1 mL·min-1. The fractions collected were treated with derivatization and separated by Gas chromatography. Use the capillary column with 5% phenyl-95%methylpolysiloxane as stationary liquid for analysis, the inlet temperature was 290 ℃, the detector temperature was 290 ℃, using programmed heating, and use helium as the carrier gas. Results:the order of sterols in soybean oil from high to low is β-sitosterol, rape oil sterol and soybean sterol, the sum of the three sterols is more than 85% of the tatal sterols; the order of sterol components in olive oil form high to low is β-sitosterol, rape oil sterol and sitosterol, the sum of these three sterol components accounts for 93% of the total sterol. Conclusion: This method is good to determine the sterol composition in pharmaceutical lipid excipients, different types of excipients have different sterol composition and proportion, it can be used for oil identification and adulteration of the judgment.

Key words: font-size:medium, ">Pharmaceutical lipid excipient; Soybean oil; Olive oil; Sterol composition

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