摘要
目的建立玉竹中4种高异黄烷酮Ⅰ,Ⅲ,Ⅳ,Ⅴ的二次层析薄层色谱(TLC)快速鉴别方法,并评价20批不同产地玉竹的质量差异。方法分别将高异黄烷酮Ⅰ,Ⅲ,Ⅳ,Ⅴ对照品与供试品溶液点于同一GF254薄层板,先后用二氯甲烷-甲醇-甲酸(150∶5∶3,V/V/V)与石油醚-乙酸乙酯(3∶2,V/V)层析展开,立即用三氯化铁试液显色与检视。结果4种对照品的TLC斑点分别与样品主斑点的位置及颜色一致;方法学验证显示,玉竹中其他成分对4种高异黄烷酮检测结果无影响;高异黄烷酮Ⅰ,Ⅲ,Ⅳ,Ⅴ的检测限(LOD)分别为2,2,1,1μg;高异黄烷酮Ⅲ,Ⅴ的TLC主斑点在1 h后颜色与大小均发生改变,高异黄烷酮Ⅰ,Ⅳ在24 h内相对稳定。20批市售玉竹中有10批4种高异黄烷酮均被检出,有7批均未被检出。结论该方法简便快速、灵敏度较高、专属性较强,可作为玉竹中4种高异黄烷酮的快速鉴别方法。
Objective To establish a secondary thin layer chromatography(TLC)identification method of four homoisoflavanones(Ⅰ,Ⅲ,Ⅳ,Ⅴ)from Polygonati odorati rhizoma and to evaluate the quality of 20 batches of Polygonati odorati rhizoma from different places of origin.Methods Reference substancesⅠ,Ⅲ,Ⅳ,Ⅴand sample solutions were separately spotted on the same GF254 thin-layer plate separately,dichloromethane-methanol-formic acid(150∶5∶3,V/V/V)and petroleum ether-ethyl acetate(3∶2,V/V)were used as developing solvents,separately.The ferric chloride test solution was used for color development and inspection immediately.Results The position and color of the main spot of the reference substances were in line with that of the samples.Methodology validation experiments showed that other components in Polygonati Odorati Rhizoma had no effect on the detection results of four homoisoflavanones;the detection limits(LOD)ofⅠ,Ⅲ,ⅣandⅤwere 2,2,1 and 1μg,respectively;the color and size of TLC main spots ofⅢand V changed after 1 h,I and IV were relatively stable within 24 h.Among the 20 batches of Polygonati odorati rhizoma,all the four homoisoflavanones were detected in 10 batches and none of the four homoisoflavanones was detected in 7 batches.Conclusion The method is simple,rapid,sensitive and specific.It can be used for the rapid identification of four homoisoflavanones in Polygonati Odorati Rhizoma.
作者
张颖
白晶
吕振
瞿志杰
李美丽
徐涛
李莉
ZHANG Ying;BAI Jing;LYU Zhen;QU Zhijie;LI Meili;XU Tao;LI Li(School of Pharmacy,Harbin University of Commerce,Pharmaceutical Engineering Technology Research Center,Harbin,Heilongjiang,China 150076;School of Pharmacy,Qiqihar Medical University,Qiqihar,Heilongjiang,China 161006)
出处
《中国药业》
CAS
2020年第7期105-109,共5页
China Pharmaceuticals
基金
齐齐哈尔医学院院内科研基金[QY2016M-01]。
关键词
玉竹
高异黄烷酮
二次层析薄层色谱
质量控制
中药材鉴定
Polygonati Odorati Rhizoma
homoisoflavanones
secondary thin layer chromatography
quality control
identification of Chinese medicine herbs
