玄参滴丸制备工艺及质量标准研究

Study on Preparation Technology and Quality Standard of Xuanshen Dropping Pills

目的确定玄参滴丸最佳制备工艺并制定其质量标准。方法以滴丸的溶散时限、外观及丸重变异系数作为综合评定指标，对玄参提取物与基质的比例、基质配比（PEG4000：PEG6000）、药液温度及滴制过程中滴速、滴距、冷凝液温度进行正交试验设计，优选出滴丸最佳成型工艺及滴制工艺。采用TLC对玄参滴丸进行定性鉴别，超高效液相色谱法（UPLC）测定玄参滴丸中哈巴俄苷的含量。色谱柱：ACQUITYUPLCBEHC18柱（2．1mm×100mm，5um）；流动相：乙腈-1％醋酸（31：69）；柱温：35℃；流速：0．2mL·min-1；检测波长：278am。结果以药物-基质（1：3），PEG4000-PEG6000（4：1），药液温度90℃，冷凝液为二甲基硅油和液体石蜡混合液为最佳成型工艺；滴速（20±21滴·min-1，滴距3cm，冰水浴冷却为最佳滴制工艺。TLC可以很好地鉴别滴丸中的主要成分，哈巴俄苷在0．010～0．040μg内呈良好的线性关系，r=0．9999，平均回收率为99．2％，RSD为0．87％。结论本试验制得的滴丸溶散时限、外观及丸重均符合质量要求，制备方法简便可行。含量测定方法操作简便、专属性强、重复性好、结果准确可靠，可用于玄参滴丸的质量控制。

OBJECTIVE To establish an optimum preparation technology and the method for quality control of Xuanshen dripping pills. METHODS Orthogonal test was applied to optimize the preparation with the choice of substrate, its proportion of substrate to drug, the drug and refrigerant temperature, dropping speed and distance to make dissolution time, appearance and weight variation up to grade. Using TLC to identify the dr/pping pills, harpagoside in dripping pills was determined by UPLC. Using ACQUITY UPLC BEH C18 column （2.1 mm × 100 mm, 5μm）, the mobile phase was acetonitrile- 1% ethylic acid （31 ： 69）, the column temperature was 35℃, the flow rate was 0.2 mL.min-1 and the detection wavelength was 278 nm. RESULTS The optimum pills preparation was the ratio of PEG4000 to PEG6000 （4 ： 1） and drug to substrate （1 ： 3）. Drug temperature was 90℃. The mixed liquid of dimethicone and liquid paraffin was refrigerant. Drug was dropped into the refrigerant of 0℃ by （20±2） dropping per minute （freeze-pillar height 3 cm）. The herbs could be identified by TLC. For harpagoside, the linear range was 0.010-0.040μg（r=0.999 9）, and the average recovery was 99.2%, RSD was 0.87%. CONCLUSION The good quality pills can be produced through this process with the simple and reliable method. The determination method is simple, specific,reproducible and accurate, and can be applied to the quality control for the Xuanshen dripping pills.