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药用辅料大豆油、橄榄油中甾醇组分的检测及分析

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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.
Determination and Analysis of Sterols in Pharmaceutical Lipid Excipients Soybean Oil and Olive Oil
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 wave-length,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 compo-nents 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 adultera-tion of the judgment.

Pharmaceutical lipid excipientSoybean oilOlive oilSterol composition

李沫、黄海、徐万魁

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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

油脂类辅料 大豆油 橄榄油 甾醇组成

2024

中国药物评价
国家食品药品监督管理局信息中心

中国药物评价

影响因子:1.09
ISSN:2095-3593
年,卷(期):2024.41(6)