目的:建立一种微柱离心方法测定紫杉醇脂肪乳包封率。方法:采用Sephadex G-50微柱,分别以适量体积的水及乙醇为洗脱液分离脂肪乳中的包封药物和游离药物。通过考察洗脱过程中紫杉醇及脂肪乳中油相成分大豆油的含量(紫杉醇的含量测定采用HPLC法,大豆油的含量测定采用HPLC-ELSD法),并以外加法制备的包封不完全的紫杉醇脂肪乳的洗脱曲线确立包封药物和游离药物的分界点,确定了最终的洗脱方式及洗脱液用量:以1 m L水,共洗3次将脂肪乳中包封药物完全洗脱,以3 m L乙醇,共洗2次将脂肪中游离药物完全洗脱。并以方法的回收率和重复性,对方法进行了验证。最终以建立的方法测定了3批紫杉醇脂肪乳样品的包封率。结果:微柱离心法能有效实现紫杉醇脂肪乳中包封药物和游离药物的分离。方法的回收率为100.4%,RSD为0.60%(n=9);重复性为99.4%,RSD为0.58%(n=5)。3批样品的包封率分别为99.2%、99.3%、99.5%。结论:该法操作简便,回收率高,重复性好,能区分不同包封情况的紫杉醇脂肪乳,测定结果准确可靠。 OBJECTIVE: To establish a microcentrifuge method for the determination of paclitaxel liposome entrapment efficiency. Methods: The Sephadex G-50 microcolumn was used to separate the encapsulated drugs and free drugs from the fat emulsion respectively with an appropriate volume of water and ethanol. By investigating the content of soybean oil in the oil phase of paclitaxel and fat emulsion during the elution process (the content of paclitaxel was determined by HPLC and the content of soybean oil was determined by HPLC-ELSD), and the incompletely encapsulated paclitaxel fat The elution curve of the milk establishes the cut-off point between the encapsulated drug and the free drug, and determines the final elution method and the amount of the eluent: completely washing the encapsulated drug in the fat emulsion with 1 m L of water for a total of 3 times, With 3 m L of ethanol, a total of 2 times to wash the fat free drug completely. The method was validated by the recovery rate and repeatability of the method. The encapsulation efficiency of three batches of paclitaxel fat emulsion samples was determined by the established method. Results: Microcolumn centrifugation can effectively separate encapsulated drug and free drug in paclitaxel fat emulsion. The recovery was 100.4% with a RSD of 0.60% (n = 9), reproducibility of 99.4%, and RSD of 0.58% (n = 5). The encapsulation efficiencies of the three batches of samples were 99.2%, 99.3% and 99.5%, respectively. Conclusion: The method is simple and convenient, high recovery, good repeatability, can distinguish paclitaxel fat emulsion with different encapsulation conditions, the determination results are accurate and reliable.