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目的:研究异亚丙基莽草酸脂质体含量和包封率的测定方法,建立一套准确度好、简便可行的质控方案。方法:采用Agilent Eclipse Plus C18色谱柱(4.6 mm×100 mm,3.5μm),流动相乙腈-0.05%磷酸溶液(10∶90),检测波长220 nm,流速1.0 mL·min-1,柱温30℃,进样量20μL。采用HPLC测定脂质体中异亚丙基莽草酸的含量;比较超滤法、凝胶色谱法和透析法用于包封率的测定。结果:异亚丙基莽草酸脂质体采用4倍量甲醇破乳并高速离心沉淀后,取上清液进行测定,药物专属性良好,线性范围1.004～150.6 mg·L-1(r=0.999 9),加样回收率(102.01±1.18)%,准确度和精密度良好,异亚丙基莽草酸对照品溶液于6 h内稳定;超滤法、葡聚糖凝胶法及透析法测得的包封率分别为(92.96±1.91)%,(91.23±2.23)%,(73.66±7.10)%。结论:所建立的HPLC稳定可靠、准确度良好,可用于异亚丙基莽草酸脂质体的质量控制和体外分析;超滤法测定包封率简便快捷、测定结果与凝胶色谱法相当,可作为本品包封率测定的常规方法;透析法由于测定条件的限制,其测定结果受脂质体溶液稳定性、药物在脂质体中存在状态的影响较大,可能会造成测定结果偏低。
OBJECTIVE: To study the determination of the content and entrapment efficiency of isopropylidene shikimic acid liposomes, and to establish a set of quality control scheme with good accuracy and simplicity. Methods: Agilent Eclipse Plus C18 column (4.6 mm × 100 mm, 3.5 μm) was used. The mobile phase was acetonitrile-0.05% phosphoric acid solution (10:90). The detection wavelength was 220 nm and the flow rate was 1.0 mL · min- ℃, injection volume 20μL. The content of isopropylidene shikimic acid in liposomes was determined by HPLC. The entrapment efficiency was determined by ultrafiltration, gel chromatography and dialysis. Results: The isopropylidene shikimic acid liposomes were disintegrated with 4 times methanol and centrifuged at high speed. The supernatant was used for determination. The drug specificity was good. The linear range was 1.004-150.6 mg · L -1 (r = 0.999 9). The recovery rate was (102.01 ± 1.18)%, and the accuracy and precision were good. The isopropylidene shikimic acid reference solution was stable within 6 h. The ultrafiltration, dextran gel and dialysis methods The entrapment efficiencies were (92.96 ± 1.91)%, (91.23 ± 2.23)% and (73.66 ± 7.10)%, respectively. Conclusion: The established HPLC is stable and reliable with good accuracy and can be used for the quality control and in vitro analysis of isopropylidene shikimic acid liposomes. The ultrafiltration method is simple and rapid in determination of entrapment efficiency, and the determination results are comparable with those of gel chromatography. Can be used as the conventional method of determination of encapsulation efficiency; dialysis method due to the determination of the limitations of the determination of the stability of the results of the liposome solution, the presence of drugs in the liposomes greater impact may result in the determination of partial low.