前列承气片的质量标准提升研究

Improvement of quality standard of Qianliechengqi Tablet

目的优化和完善前列承气片的质量标准。方法使用显微鉴别法检验样品中原粉入药的药材,使用薄层色谱法鉴别药品中大黄、防己、丹参,对方中君药虎杖中虎杖苷采用高效液相色谱法进行含量测定,使用艾杰尔Innoval C18色谱柱,以乙腈-水(23∶77)做为流动相洗脱,检测波长为306 nm。结果显微鉴别检测到大黄中簇晶、丹参中木栓细胞和纤维状石细胞、厚朴中石细胞;丹参、枳实、大黄、防己的薄层色谱鉴别斑点清晰,分离度较好,且阴性对照无干扰;虎杖苷在进样量0.066~0.330μg范围内线性关系良好,相关系数r=0.999 7,精密度、稳定性、重复性试验的RSD <2.0%;加样回收率为96.65%(RSD <2.0%)。结论定性定量方法简便、结果准确可靠、专属性强,所建标准可用于前列承气片的质量控制。

Objective To optimize and consummate the quality standard of Qianliechengqi Tablet. Methods Microscopic identification was used to identify the medicine prescribed as powder. TLC was used to qualify the identification of Rhei Radix et Rhizoma, Stephaniae Trtrandrae Radix,Salviae Miltiorrhizae Radix et Rhizoma. HPLC was used to determine the contents of polydatin. The sample was separated on a Agela Innoval C18(4.6×260 mm,5μm)column by a elution using acetonitrile: distilled water(27∶33)as the mobile phase and detection wavelength was set at 306 nm. Results Microscopic identification has detected Cluster crystals in Rhei Radix et Rhizoma, fibrous stone cells in Magnoliae Officinalis Cortex, cork cells and fibrous stone cells in Salviae Miltiorrhizae Radix et Rhizoma. TLC spots were clear and well-separated without negative interference.HPLC experiment showed good linear relationships at the ranges of 0.066 ~ 0.330μg for polydatin(r = 0.999 7). RSDs of precision, stability and reproducibility tests were all lower than 2.0%. The sample recovery was 96.65%(RSD < 2.0%). Conclusion The method is simple,accurate and reliable with good precision.It can be used for the quality control of Qianliechengqi Tablet.