薄层色谱法鉴别槐枝及高效液相色谱法测定其中芦丁含量  

Identification of Sophora Japonica by thin layer chromatography and determination of rutin by high performance liquid chromatography

作　　者：于姗姗 王云 李敏 张秋红 Yu Shanshan;Wang Yun;Li Min;Zhang Qiuhong(Jinan Supervision and Inspection Center for Food and Drug Control,Jinan 250102,China)

机构地区：[1]济南市食品药品检验检测中心,济南250102

出　　处：《化学分析计量》2021年第10期7-11,共5页Chemical Analysis And Meterage

基　　金：山东省药品监督管理局山东省中药材及饮片标准研究(2020–138、2020–139)。

摘　　要：建立槐枝的薄层色谱(TLC)鉴别及高效液相色谱(HPLC)法测定其中芦丁含量的方法。样品中加入石油醚(30~60℃)脱色,然后用甲醇超声提取,以乙酸乙酯-甲醇-甲酸-水(体积比为8∶1∶1∶1)为展开剂,建立槐枝的薄层色谱鉴别方法。选用Kromasil C18柱(250 mm×4.6 mm,5μm)为分离柱,流动相为甲醇-1%冰醋酸溶液(体积比为32∶68),流量为1.0 mL/min,柱温为36℃,采用HPLC法测定芦丁含量,检测波长为257 nm。芦丁的质量在45.3~226.5 ng范围内与色谱峰面积具有良好的线性关系,相关系数为1.000,方法检出限为1.54 ng。测定结果的相对标准偏差为1.6%(n=6),样品加标回收率为98.7%~102.2%。所建立的薄层色谱鉴别方法及高效液相色谱法测定其中芦丁含量的方法可以有效控制槐枝的质量。A method of identification of Sophora japonica by thin layer chromatography(TLC)and determination of rutin by high performance liquid chromatography(HPLC)was established.Petroleum ether(30-60℃)was added to the sample for decolorization,and then ultrasonic extraction with methanol.Ethyl acetate-methanol-formic acid-water(volume ratio was 8∶1∶1∶1)was used as the developer to establish the TLC identification method of Sophora japonica.Kromasil C18 column(250 mm×4.6 mm,5μm)was used as separation column,the mobile phase was methanol-1%glacial acetic acid solution(volume ratio was 32∶68),the flow rate was 1.0 mL/min,the column temperature was 36℃,the rutin content was determined by HPLC,and the detection wavelength was 257 nm.The mass of rutin had a good linear relationship with the chromatographic peak area in the range of 45.3-226.5 ng,the correlation coefficient was 1.000,and the detection limit was 1.54 ng.The relative standard deviation of determination results was 1.6%(n=6),and the recoveries of the standard addition were 98.7%-102.2%.The established TLC identification method and HPLC method can effectively control the quality of Sophora japonica.

关 键 词：槐枝 芦丁 薄层色谱 高效液相色谱法 

分 类 号：O657.7[理学—分析化学]