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纸质出版日期:2013
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曲昌海, 尹兴斌, 张慧, 等. 异亚丙基莽草酸脂质体的包封率测定方法比较[J]. 中国实验方剂学杂志, 2013,19(1):21-24.
QU Chang-hai, YIN Xing-bin, ZHANG Hui, et al. Comparative Study of Entrapment Efficiency Determination for Isopropylidene Shikimic Acid Liposome[J]. Chinese journal of experimental traditional medical formulae, 2013, 19(1): 21-24.
曲昌海, 尹兴斌, 张慧, 等. 异亚丙基莽草酸脂质体的包封率测定方法比较[J]. 中国实验方剂学杂志, 2013,19(1):21-24. DOI:
QU Chang-hai, YIN Xing-bin, ZHANG Hui, et al. Comparative Study of Entrapment Efficiency Determination for Isopropylidene Shikimic Acid Liposome[J]. Chinese journal of experimental traditional medical formulae, 2013, 19(1): 21-24. DOI:
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
3.5 μm)
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20 μL。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 establish a simple
feasible and precise quality control strategy for determination of concentration and entrapment efficiency of isopropylidene shikimic acid liposome. Method: Chromatographic conditions were: Agilent Eclipse Plus C18 column (4.6 mm×100 mm
3.5 μm)
column temperature of 30℃
mobile phase of acetonitrile-0.05% phosphoric acid solution(10:90)
flow rate of 1.0 mL·min-1
injection volume of 20 μL and detection wavelength at 220 nm.The content of ISA in liposomes was determined by HPLC;Encapsulation efficiency was determined by ultrafiltration
gel chromatography and dialysis method
respectively
and results were compared with each other. Result: After demulsification by adding 4 times the amount of methanol into ISA liposome and high speed centrifugal sedimentation
supernatant was used to determine
determination results showed a good specificity
precision and accuracy
regression equation showed a good linearity (r=0.999 9) within range of 1.004-150.6 mg·L-1
recovery was (102.01±1.18)%
reference substance solution of ISA was stable in 6 h;Entrapment efficiency of ISA liposome determined by ultrafiltration method
gel permeation method and dialysis method were (92.96±1.91)%
(91.23±2.23)%
(73.66±7.10)%
respectively. Conclusion: This established HPLC method was stable and reliable
it could be used for quality control and in vitro analysis;In determination of encapsulation efficiency
ultrafiltration method was simple and efficient
its results were close to gel permeation chromatography;Due to limit of measurement conditions
determination result of dialysis method might be lower for its time-consuming process and higher temperature
and also depending on stability of liposome solution and existence state of drugs in liposome.
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