正交试验优选心舒滴丸的制备工艺及含量测定方法研究

目的:优选心舒滴丸的制备工艺并建立其含量测定方法。方法:以溶散时间、丸重差异变异系数、综合得分为考察指标,清膏与基质质量比、PEG4000与PEG6000质量比、滴速、药液温度为考察因素,通过正交试验优选心舒滴丸的制备工艺。采用高效液相色谱法(HPLC)测定人参皂苷Rg1、Rb1、Re的含量。色谱柱为Diamond C18(250 mm×4.6 mm,5μm),流动相为乙腈-水(梯度洗脱),流速为1 ml/min,检测波长为203 nm,柱温为30℃。结果:优选制备工艺为清膏与基质质量比为1∶3,PEG4000与PEG6000质量比为1∶1.5,滴速为50滴/min,药液温度为80℃。心舒滴丸丸重差异变异系数为1.72%,平均溶散时间为3.5 min。人参皂苷Rg1、Rb1、Re的进样量分别在1.005⁶.030、1.1026.030、1.102⁶.612、1.0336.612、1.033⁶.198μg范围内与各自峰面积积分值呈良好线性关系(r=0.999 7,n=6)。人参皂苷Rg1、Rb1、Re的重复性、稳定性、精密度、加样回收率试验的RSD<2%。结论:本研究优选出的心舒滴丸制备工艺合理、稳定、可行,含量测定方法专属性强,可用于该制剂的质量控制。

Optimization of Preparation Technology of Xinshu Dripping Pills by Orthogonal Test and Study on the Meth- od for Content Determination

OBJECTIVE： To optimize the preparation technology of Xinshu dripping pills, and to set up a method for content determination. METHODS： Using dissolving time, the coefficent of varation of pill weight difference and comprehensive score as index, the preparation technology of Xinshu dripping pills was optimized by orthogonal test with ratio of plaster to matrix, ratio of PEG4000 to PEG6000, dripping speed and solution temperature as factors. The contents of ginsenoside Rg1, Rb, and Re were deter- mined by HPLC. The determination was performed on Diamond C18 column （250 mm×4.6 mm, 5 μm） with mobile phase consisted of acetonitrile-water （gradient elution） at the flow rate of 1 ml/min. The detection wavelength was set at 203 nm, and column tem- perature was 30 ℃. RESULTS ： Optimal techonolgy was as follows ： the mass ratio of ointment to stroma 1 ： 3, the mass ratio of PEG4000 and PEG6000 1 ： 1.5, the dropping speed 50 drops of/min, the temperature of the medicine liquid 80 ℃. The weight differ- ence coefficient of variation of xinshu pills was 1.72%, the average time to dissolve powder is 3.5 min and average dissolving time was 3.5 min. The linear range was 1.005-6.030 μg for ginsenoside Rg1（r=0.999 7,n=6）, 1.102-6.612 μg for ginsenoside Rb1（r= 0.999 7, n=6）and 1.033-6.198 gg for ginsenoside Re（r=0.999 7,n=6）, respectively. RSD of reproducibility, stability, precision and recovery tests of ginsenoside Rg1, Rb1 and Re were all lower than 2 %. CONCLUSIONS： The preparation technology is reason- able and feasible, and the determination method can be used for the quality control of Xinshu dripping pills.