基于HPLC-ELSD法的银柴胡中甾醇类成分含量测定  

Content determination of sterols in Radix Stellariae lanceolatae by HPLC-ELSD

作　　者：王秀芬[1] 李静[1] 方光明 马学琴[2] WANG Xiufen;LI Jing;FANG Guangming;MA Xueqin(Ningxia Polytechnic College,Yinchuan 750021,China;Ningxia Medical University,Yinchuan 750001,China)

机构地区：[1]宁夏职业技术学院,银川750021 [2]宁夏医科大学,银川750001

出　　处：《西北药学杂志》2021年第4期551-554,共4页Northwest Pharmaceutical Journal

基　　金：宁夏自然科学基金项目(编号:2019AAC03248)。

摘　　要：目的建立银柴胡药材中甾醇类成分α-菠甾醇和豆甾-7-烯醇的含量测定方法。方法采用高效液相蒸发光散射检测法(HPLC-ELSD),SHIMADZU Shim-pack GIST C 18色谱柱(250 mm×4.6 mm,5μm);流动相为甲醇-水(98∶2);流速:1 mL·min^(-1);柱温:40℃;检测器漂移管温度:70℃;喷雾器温度:30℃;载气流速:1.6 L·min^(-1);进样量:50μL。结果在该色谱条件下,α-菠甾醇和豆甾-7-烯醇分离完全,质量浓度分别在10.77~43.09、8.70~81.20μg·mL-1范围内线性关系良好;α-菠甾醇的检测限、定量限分别为0.1075、0.4300μg,平均回收率(n=6)为104.04%,RSD值为2.56%;豆甾-7-烯醇的检测限、定量限分别为0.0174、0.0870μg,平均回收率(n=6)为96.50%,RSD值为2.12%;二者精密度、重复性、稳定性实验的RSD值均小于3%。结论建立的含量测定方法简便、灵敏、重复性好,能够实现对银柴胡药材中甾醇类成分的质量控制。Objective To establish a method for the content determination of sterols ofα-spinasterol and stigmasterol-7-enol in Radix Stellariae lanceolatae.Methods High-performance liquid chromatography-evaporative light-scattering detector(HPLC-ELSD)was used.The samples were separated on a SHIMADZU Shim-pack GIST C 18(250 mm×4.6 mm,5μm)column at 40℃.The mobile phase was methanol-water(98∶2),and the flow rate was 1 mL·min^(-1).The drift tube temperature was 70℃,the sprayer temperature was 30℃,the carrier gas flow rate was 1.6 L·min^(-1),and the injection volume was 50μL.Results Under the established chromatographic conditions,α-spinasterol and stigmasterol-7-enol were separated completely.The linear ranges were 10.77-43.09 and 8.70-81.20μg·mL-1 respectively.The detection limit and quantitation limit ofα-spinasterol were 0.1075 and 0.4300μg,respectively,and the average recovery(n=6)was 104.04%with RSD of 2.56%.The detection limit and quantitation limit of stigmasterol-7-enol were 0.0174 and 0.0870μg,respectively,and the average recovery(n=6)was 96.50%with RSDs of 2.12%.The RSDs of precision,repeatability and stability tests were less than 3%.Conclusion The method is simple,sensitive and reproducible,which can be used for the quality control of sterols in Radix Stellariae lanceolatae.

关 键 词：银柴胡 甾醇类成分 高效液相蒸发光散射检测法(HPLC-ELSD) 含量测定 

分 类 号：R927.2[医药卫生—药学]