苦参碱胃内漂浮颗粒的质量标准建立及稳定性考察

目的:建立苦参碱胃内漂浮颗粒的质量标准,并对其稳定性进行初步考察。方法:采用高效液相色谱法测定制剂中苦参碱的含量。色谱柱为ZORBAX Eclipse XDB-C18(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸溶液(70∶30,V/V;用三乙胺调p H至6.0),检测波长为220 nm,流速为1.0 ml/min,柱温为30℃,进样量为5μl。通过影响因素试验考察制剂的初步稳定性。结果:苦参碱的质量浓度在0.004 95⁰.316 8 mg/ml范围内与峰面积积分值呈良好线性关系(r=0.999 8);精密度、稳定性、加样回收率的RSD<2.0%。3批样品2 h/8 h释放量分别为标示量的27.82%/82.18%、25.27%/84.21%、26.34%/86.99%;制剂在无包装保护的情况下,于高温(60℃)、强光[(4 500±500)lx]、高湿度[(90±5)%]环境中放置10 d不稳定。结论:苦参碱胃内漂浮颗粒制备工艺简单,稳定易控,缓释效果和漂浮性良好,制备的样品符合制剂质量要求;初步稳定性试验结果提示本品应防潮、避光和常温贮藏。

Quality Criteria Establishment and Stability Evaluation of Matrine Gastric Floating Particles

OBJECTIVE： To establish the quality criteria for Matrine gastric floating particles and preliminarily evaluate their stability. METHODS： The content of matrine was determined by HPLC. The determination was performed on ZORBAX Eclipse XDB-C18 （250 mm×4.6 mm, 5 μm） column with mobile phase consisted of methanol-0.1% phosphoric acid （70：30, V/V; pH value adjusted to 6.0） at the flow rate of 1.0 ml/min. The detection wavelength was set at 220 nm and column temperature was 30 %. The sample size was 5 μl. The initial stability of the preparation was evaluated through influential factor test. RESULTS：The linear range of matrine was 0.004 95-0.316 8 mg/ml （r=0.999 8）. RSD of precision, stability and recovery tests were all less than 2.0%. The release amount of 3 batches of samples within 2 h/8 h accounted for 27.82%/82.18%, 25.27%/84.21% and 26.34%/86.99% of the labeled amount, respectively. Under the circumstance of unpackaged, samples were not stable if placed for ten days under the high temperature （60 ℃ ）, strong light [ （4 500 ± 500） 1x] and high humidity [ （90 ± 5） % ]. CONCLUSIONS： The preparation technology of Matrine gastric floating particles is simple, stable and easy to control. Matrine gastric floating particles are of good sustained-release effect and floatability. Prepared particles have met quality demand. Storage in dry, preferably dark places and at room temperature is recommended.