HPLC法测定醋酸曲普瑞林微球的载药量及包封率

HPLC Determination of Drug Loading and Encapsulated Efficiency of Triptorelin Acetate Microspheres

目的建立HPLC法测定醋酸曲普瑞林微球的载药量和包封率的方法。方法色谱柱为Phenomenex Kinetex? EVO C18(150 mm×4.6 mm, 5μm);流动相为0.05 mol·L^(-1)磷酸溶液(用三乙胺调节pH值至3.5)-乙腈(78∶22);柱温35℃;流速为1.0 mL·min^(-1);检测波长为220 nm。结果空白溶剂、空白微球及供试品溶液中其他杂质色谱峰对主峰曲普瑞林的测定无干扰,曲普瑞林与前后相邻已知杂质峰分离度大于1.5;曲普瑞林浓度范围在44.5~133.6μg·mL^(-1)线性良好,相关系数为0.999 9(n=5);定量限为0.16μg·mL^(-1);50%浓度回收率为100.1%,100%浓度回收率为100.5%,150%浓度回收率为100.5%,RSD为0.5%;重复性RSD为0.8%。结论高效液相色谱方法准确、可靠、专属性强、耐用,可用于醋酸曲普瑞林缓释微球中药物含量的测定和包封率的测定,为制剂的质量控制提供方法。

OBJECTIVE HPLC method to established a HPLC method for the determination of drug loading and encapsulated efficiency of triptorelin acetate microspheres. METHODS A Phenomenex Kinetex? EVO C18(150 mm×4.6 mm, 5 μm) column was adopted with a mobile phase of 0.05 mol·L^(-1) phosphoric acid solution(adjust pH to 3.5 with triethylamine)-acetonitrile(78∶22).The flow rate was 1.0 mL·min^(-1).The detection wavelength was set at 220 nm and the column temperature was 35 ℃. RESULTS The blank solvent, blank microspheres and other impurities in samples did not interfere with the determination of triptorelin.The resolution between triptoreline and adjacent impurity peaks were more than 1.5.The standardcurve of triptorelin was at good linear in the range of 44.5-133.6 μg·mL^(-1).The correlation coefficient was reach 0.999 9(n=5).The quantitation limit was 0.16 μg·mL^(-1).The recovery rate of concentration of 50% was 100.1%, and the recovery rate of concentration of 100% was 100.5%.The recovery rate of concentration of 150% was 100.5%.And RSD was 0.5%,the RSD of repeatability was 0.8%. CONCLUSION The method of HPLC is accurate, reliable, specific and durable.It can be used to determinate the drug loading and encapsulated efficiency of triptorelin acetate microspheres and for quality control of microspheres.