摘要
目的:建立千斤拔药材的质量标准。方法:观察千斤拔药材性状和显微鉴别特征;采用薄层色谱法(TLC)对药材中染料木苷和染料木素进行定性鉴别;检查药材水分、总灰分和浸出物。采用高效液相色谱法(HPLC)测定药材中染料木苷和染料木素的含量:色谱柱为ThermoBETASILC18,流动相为乙腈-0.5%冰醋酸(梯度洗脱),流速为1.0ml/min,检测波长为261nm,柱温为25℃,进样量为10μl。结果:千斤拔和大叶千斤拔的性状和显微鉴别特征显著;染料木苷和染料木素的TLC斑点清晰,分离良好,阴性对照无干扰;药材水分为3.69%~8.37%,总灰分为1.72%~6.74%,浸出物为5.89%~19.65%。染料木苷和染料木素检测进样量线性范围分别为0.0129~2.5880、0.0046~0.9232μg(r均为0.9999);精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为99.63%~101.87%(RSD=0.82%,n=6)、97.19%~100.34%(RSD=1.23%,n=6)。结论:该标准可用于千斤拔药材的质量控制。
OBJECTIVE:To establish the quality standard of Flemingia philippinensis. METHODS:The properties and microscopiccharacteristics were observed;TLC was adopted for qualitative identification of genistin and genistein;the moisture,totalash and extract were detected;HPLC was adopted for contents determination of genistin and genistein:the column was Thermo BETASILC18 with mobile phase of Acetonitrile -0.5% glacial acetic acid(gradient elution)at a flow rate of 1.0 ml/min,the detectionwavelength was 261 nm,column temperature was 25 ℃,and the injection volume was 10 μl. RESULTS:The properties and microscopiccharacteristics of F. philippinensis and F. macrophylla showed strong specificity. TLC spots of genistin and genistein we- reclear and well separated,with no interference in negative control. The moisture was 3.69%-8.37%,total ash was 1.72%-6.74%,andextract was 5.89%-19.65%. The linear range was 0.012 9-2.588 μg for genistin(r=0.999 9)and 0.004 6-0.923 2 μg for genistein(r=0.999 9);RSDs of precision,stability and reproducibility tests were lower than 3.0% ;recoveries were 99.63% -101.87%(RSD=0.82%,n=6)and 97.19%-100.34%(RSD=1.23%,n=6). CONCLUSIONS:The method is simple,accurate and specific,and can be used for the quality control of F. philippinensis.
作者
林锦锋
李清明
朱玉芳
陈浩桉
LIN Jinfeng;LI Qingming;ZHU Yufang;CHEN Hao’an(Guangdong Institute for Drug Control,Guangzhou 510180,China;Zhongshan Institute for Food and Drug Control,Guangdong Zhongshan 528437,China)
出处
《中国药房》
CAS
北大核心
2016年第24期3400-3403,共4页
China Pharmacy
基金
国家食品药品监督管理局"进口药材标准增修订"专项课题(No.JKYC2012-2)
广东省省级科技计划项目(No.2013B040200029)