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目的建立琥珀酸甲泼尼龙(MPS)聚合物胶束的包封率测定方法。方法采用高速离心法分离MPS聚合物胶束和游离MPS;碱溶液法破坏聚合物胶束,提取MPS;RP-HPLC法测定MPS的包封率,以甲醇-10 mmol·L-1pH 3.0的KH2PO4(体积比65∶35)为流动相,C18柱(250 mm×4.6 mm,5μm)为色谱柱,柱温为35℃,流速为0.8 mL·min-1,检测波长为254 nm。结果当NaOH溶液浓度为5.0 mmol·L-1、聚合物胶束与NaOH质量比为10∶1时,NaOH可破坏聚合物胶束,并溶解MPS,得到pH为7.50的澄清溶液。按建立的包封率测定方法,MPS主峰与杂质峰分离良好,线性范围为10.12~91.08μg·mL-1(r=0.999 9,n=5),平均回收率为101.8%,RSD为1.47%,日内、日间精密度及样品稳定性均良好。采用该法测定3批MPS聚合物胶束的平均包封率为(85.35±1.02)%。结论所建立的琥珀酸甲泼尼龙(MPS)聚合物胶束包封率的测定方法简便快速,准确可靠。
Objective To establish a method for determining the entrapment efficiency of methylprednisolone succinate (MPS) polymer micelles. Methods MPS micelles and free MPS were isolated by high-speed centrifugation. The polymer micelles were destroyed by alkaline solution and MPS was extracted. The entrapment efficiency of MPS was determined by RP-HPLC. KH2PO4 with 10 mmol·L-1 pH 3.0 (65:35) as the mobile phase. The column was C18 (250 mm × 4.6 mm, 5 μm). The column temperature was 35 ℃, the flow rate was 0.8 mL · min-1 and the detection wavelength was 254 nm. Results When the concentration of NaOH solution was 5.0 mmol·L-1 and the mass ratio of polymer micelles to NaOH was 10:1, NaOH could destroy the polymer micelles and dissolve the MPS to obtain a clear solution with a pH value of 7.50. According to the established method of entrapment efficiency, the peak of MPS and impurity peaks separated well with the linear range of 10.12-91.08 μg · mL-1 (r = 0.999 9, n = 5). The average recovery was 101.8% and the RSD was 1.47% , Day, day precision and sample stability are good. The average entrapment efficiency of three batches of MPS polymer micelles by this method was (85.35 ± 1.02)%. Conclusion The method for determining the entrapment efficiency of MPS polymer micelles is simple, rapid, accurate and reliable.