复方茜蒌颗粒大叶茜草素含量测定及茜草药材TLC鉴别
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摘要
建立复方茜蒌颗粒中大叶茜草素HPLC含量测定方法及制剂中茜草药材TLC鉴别方法。(1)色谱柱为X Bridge shield Rp18(4.6×250 mm,5μm),流动相为乙腈-0.2%磷酸水(88∶12),流速为1.0m L·min~(-1),柱温为25℃,检测波长为210 nm;(2)展开剂为石油醚(60-90℃)-丙酮(4∶1.5)。(1)在该色谱条件下,大叶茜草素在20-100μg·m L~(-1)范围内线性关系良好(r=0.9997);平均回收率为99.06%,(RSD=1.34%)。(2)薄层色谱中检出茜草药材的特征斑点,与对照品及对照药材色谱相应的位置上,显相同颜色的斑点,阴性对照品无干扰斑点检出。本方法操作简便,能有效地鉴别制剂中茜草药材成分,可用于复方茜蒌颗粒的质量控制。
To establish a quantitative HPLC method for the determinnation of Rubimaillin from Qi Qian compond granules,and a TLC identification method for Radix Rubiae in preparations.( 1) The determination was carried out on a X Bridge shield Rp18 column at 25℃ with acetonitrile-0. 2%phosphoric acid( 88 ∶ 12) as mobile phase and detection wavelength was set at 210 nm,the flow rate was 1. 0 m L·min~(-1).( 2) The developing solvent was petroleum ether( 60-90℃)-acetone( 4 ∶ 1. 5).Mollugin showed a good linear relationship with the range of 20-100 μg · m L~(-1)(r = 0. 9997). The average recovery rate was 99. 06%(RSD = 1. 34%).This method repeatable with easy operation,it can be used for the quality control of compond Qi Qian granules.
To establish a quantitative HPLC method for the determinnation of Rubimaillin from Qi Qian compond granules,and a TLC identification method for Radix Rubiae in preparations.( 1) The determination was carried out on a X Bridge shield Rp18 column at 25℃ with acetonitrile-0. 2%phosphoric acid( 88 ∶ 12) as mobile phase and detection wavelength was set at 210 nm,the flow rate was 1. 0 m L·min~(-1).( 2) The developing solvent was petroleum ether( 60-90℃)-acetone( 4 ∶ 1. 5).Mollugin showed a good linear relationship with the range of 20-100 μg · m L~(-1)(r = 0. 9997). The average recovery rate was 99. 06%(RSD = 1. 34%).This method repeatable with easy operation,it can be used for the quality control of compond Qi Qian granules.
引文
[1]国家药典委员会.中华人民共和国药典2015版一部[S].北京:中国医药科技出版社,2015,6.
[2]浦益琼,王冰,张彤,等.茜草提取物中大叶茜草素测定的方法研究[J].中国实验方剂学杂志,2012,6(18):94-96.
[3]方乐敏,杨骏,刘云,等.复方茜草片质量标准的研究[J].中成药,2016,38(6):1293-1297.
[4]刘广,齐娜,徐本明.大叶茜草素在甲醇溶液中的稳定性研究[J].华西药学杂志,2010,25(3):318.
[2]浦益琼,王冰,张彤,等.茜草提取物中大叶茜草素测定的方法研究[J].中国实验方剂学杂志,2012,6(18):94-96.
[3]方乐敏,杨骏,刘云,等.复方茜草片质量标准的研究[J].中成药,2016,38(6):1293-1297.
[4]刘广,齐娜,徐本明.大叶茜草素在甲醇溶液中的稳定性研究[J].华西药学杂志,2010,25(3):318.