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目的研究复方木尼孜其颗粒中骆驼蓬子的质量控制方法。方法分别以骆驼蓬碱(HAL)和去氢骆驼蓬碱(HAR)为对照,建立复方木尼孜其颗粒中骆驼蓬子的薄层色谱鉴别及HPLC含量测定方法。薄层色谱:以硅胶HSGF254为薄层板,乙酸乙酯-甲醇-氨水(10∶1.5∶0.5)为展开剂;HPLC条件:采用反相HPLC色谱柱,以乙腈-醋酸铵缓冲盐(22∶78)为流动相,流速1.0 ml/min,柱温为30℃,检测波长为330 nm。结果复方木尼孜其颗粒的薄层色谱中HAL、HAR分离度良好,可以用于鉴别复方木尼孜其颗粒中的骆驼蓬子。含量测定方法学研究结果表明,HAL和HAR分别在0.33~104.10 mg/L和0.13~40.91 mg/L范围内呈良好的线性关系,方法平均回收率分别为97.04%和101.83%,RSD分别为2.02%和2.32%,方法的日内和日间精密度RSD均小于3%。15批复方木尼孜其颗粒样品的测定结果表明,HAL含量范围为1.62~5.04 mg/袋,平均为(2.87±0.95)mg/袋;HAR含量范围为0.87~2.22 mg/袋,平均为(1.51±0.41)mg/袋;总碱(HAL+HAR)含量范围为(2.49~7.14)mg/袋,平均为(4.38±1.33)mg/袋。结论建立的复方木尼孜其颗粒中骆驼蓬子质量控制方法灵敏、准确、重现性好、精密度高、专属性强,适用于复方木尼孜其颗粒中骆驼蓬子的质量控制。
Objective To study the quality control method of Peganum harmala in compound miznizi granule. Methods HAL and HAR were used as control to establish TLC and HPLC method for determination of Peganum harmala in Fujinumizi Granules. Thin layer chromatography: silica gel HSGF254 TLC plate, ethyl acetate - methanol - ammonia (10: 1.5: 0.5) as developing solvent; HPLC conditions: using reverse phase HPLC column with acetonitrile - ammonium acetate buffer salt 78) as the mobile phase at a flow rate of 1.0 ml / min with a column temperature of 30 ° C and a detection wavelength of 330 nm. Results The TLC and HAL, HAR of compound mizniqi particles were well resolved and could be used to identify Peganum harmala in compound mizniqi granules. The methodological determination results showed that there was a good linear relationship between HAL and HAR in the range of 0.33-104.10 mg / L and 0.13-40.91 mg / L, respectively. The average recoveries of HAL and HAR were 97.04% and 101.83%, respectively, with RSDs of 2.02 % And 2.32% respectively. The RSDs of intra-day and inter-day precision were less than 3%. The results showed that the content of HAL ranged from 1.62 to 5.04 mg / bag, with an average of (2.87 ± 0.95) mg / bag and HAR content ranged from 0.87 to 2.22 mg / bag with an average of ( 1.51 ± 0.41) mg / bag, and the content of total alkaloids (HAL + HAR) was (2.49 ~ 7.14) mg / bag with an average of (4.38 ± 1.33) mg / bag. Conclusions The established quality control method of Peganum harmala is accurate, reproducible, precise and specific. It is suitable for the quality control of Peganum harmala in the compound miznizi granules.