千斤拔药材的质量标准研究

Study on the Quality Standard of Flemingia philippinensis

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.