摘要
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 establish the quality standards of Peganum harmala in ＂Compound Muniziqi Granules＂. Methods -Taking HAL and HAR as control, to establish the quality standards of P. harmala in ＂Compound Muniziqi Granules＂ by thin-layer chromatography （TLC） and HPLC. The TLC method was developed by using mixture of ethyl acetate-methanol-ammonia （10：1.5：0.5 ） as a developing solvent on high performance silica gel precoated plate （HSGF254）. In the HPLC method, HAL and HAR was separated on a reverse phase HPLC chromatographic column with acetonitrile-ammonium acetate （22：78 ） as the mobile phase with flow rate of 1.0 ml/min, column temperature was maintained at 30℃ and the wave length was detected at 330 nm. Results The reslutes of HPLC showed that HAL and HAR displayed ideal linearity within the ranges of 0.33 - 104.10 and 0.13 - 40.91 mg/L. The average recoveries of HAL and HAR were 97.04% and 101.83% with RSD of 2.02% and 2.32%, respectively. The RSD values of intra-day and inter-day precision were less than 3%. The content of HAL in 15 batches ＂Compound Muniziqi Granules＂ fluctuates between 1.62 - 5.04 mg and HAR between 0.87 and 2.22 mg of each bag, the total alkali between 2.49 - 7.14 mg of each bag. Conclusion The method was sensitive, accurate, reproducible, and it can be used to determine and control the quality of seeds of P. harmala in ＂Compound Muniziqi Granules＂.
出处
《上海中医药杂志》
2014年第11期91-95,共5页
Shanghai Journal of Traditional Chinese Medicine
基金
国家自然基金-新疆联合基金重点项目(U1130303)
新疆维吾尔自治区科技支疆计划(指令性)项目(2013911134)
上海市国内科技合作领域资助项目(14495800200)
新疆维吾尔自治区科技计划项目(201130105-5)
