止吐六味散质量标准

Quality Standard Analysis of Zhitu Liuweisan

目的研究止吐六味散质量控制方法。方法采用显微鉴别法对止吐六味散进行粉末鉴定;依据《中华人民共和国药典》2015年版进行水分、灰分、浸出物含量测定;薄层色谱法对止吐六味散中甘草、芫荽子、小茴香和酸梨干进行定性鉴别;采用高效液相色谱(HPLC)法测定止吐六味散中甘草苷、甘草酸含量,色谱条件为Syncronis C18色谱柱(250 mm×4.6 mm,5μm),柱温:38℃,流动相:乙腈-0.05%磷酸,流速:1 mL·min-1,波长:263 nm。结果组成止吐六味散的单药,除了芫荽子,其他均有明显显微特征。止吐六味散水分含量6.89%～7.75%,灰分含量4.06%～4.40%,酸不溶性灰分含量1.24%～1.44%,水溶性浸出物含量21.17%～22.63%。甘草、芫荽子、小茴香和酸梨干薄层色谱特征明显,阴性均无干扰。甘草苷、甘草酸分别在0.06～3.00μg,0.078 4～0.392 0μg有良好线性关系。平均回收率分别为99.06%～101.90%,99.66%～100.83%。结论该实验建立的方法可靠,结果准确,可为全面评价止吐六味散的质量提供参考。

Objective To establish quality analysis of Zhitu liuweisan . Methods Zhitu liuweisan was identified by microscopic identification method.The moisture, ash, and extract of Zhitu liuweisan were determined based on the methods of Chinese pharmacopoeia (2015 edition).The thin layer chromatography was adopted to identify Radix Glycyrrhizae, Fructus Coriandri, Fructus Foeniculi, Pyrus ussuriensis Maxin .of Zhitu liuweisan .Liquiritin and glycyrrhizic acid in Zhitu liuweisan were determined by high performance liquid chromatography.The determination was performed on Syncronis C 18 (250 mm×4.6 mm, 5 μm) with mobile phase consisting of acetonitrile-0.05% phosphoric acid at flow rate of 1 mL·min -1 .The detection wave length was set at 263 nm and the column temperature was 38 ℃. Results Except Fructus Coriandri, the other herbs in Zhitu liuweisan had significant microscopic characteristics.The content of moisture was 6.89%-7.75%;the content of total ash was 4.06%-4.40%;the acid insoluble ash was 1.24%-1.44%;water extract was 21.17%-22.63%.TLC spots of Fructus Coriandri, Fructus Foeniculi, Radix Glycyrrhizae, Pyrus ussuriensis Maxin.were clear and well-separated without interference from negative control.Good linearity was obtained for liquiritin and glycyrrhizic acid within the range of 0.06-3.00 μg and 0.078 4-0.392 0 μg, respectively. The average recovery were 99.06%~101.90%,99.66%~100.83% respectively. Conclusion The methods were reliable, accurate and can be used for quality control of Zhitu liuweisan .