HPLC-ELSD法测定注射用福沙匹坦二甲葡胺中聚山梨酯80和EDTA的含量

Determination of polysorbate 80 and EDTA in Fosaprepitant Dimeglumine for Injection by HPLC-ELSD

目的建立高效液相-蒸发光散射检测器色谱法同时测定注射用福沙匹坦二甲葡胺中聚山梨酯80和乙二胺四乙酸的含量。方法采用分子凝胶为填充剂(TSK-GEL G2500PWXL,7.8 mm×300 mm,7μm);以0.02mol·L^(-1)醋酸铵溶液-乙腈(90∶10)为流动相;柱温为30℃;流速为0.6 m L·min^(-1);蒸发光散射检测器,其参数设置:漂移管温度为110℃,氮气流速为2.6 L·min^(-1),撞击器模式为关。结果聚山梨酯80在418.80~1 256.40μg·m L^(-1)浓度范围内呈良好的对数线性关系(r=0.999 3),平均回收率为98.55%,RSD为0.99%;乙二胺四乙酸在100.56~301.68μg·m L^(-1)浓度范围内呈良好的对数线性关系(r=0.999 9),平均回收率为100.13%,RSD为0.52%。结论本方法简便,快速,准确,灵敏度高,重复性好,可用于注射用福沙匹坦二甲葡胺中聚山梨酯80和EDTA含量的测定。

Objective To establish an HPLC -ELSD for the determination of polysorbate 80 and EDTA in Fosaprepi-tant Dimeglumine for Injection.Methods The chromatographic analysis was carried out on a TSK -GEL G2500PWXL (7.8 mm ×300 mm,7 μm).The mobile phase consisted of 0.02 mol·L -1 ammonium acetate -acetonitrile(90∶10)with the flow rate of 0.6 mL·min -1 .The column temperature was 30 ℃.The drift tube temperature of ELSD was 110 ℃ and gas flow rate of nitrogen was 2.6 L · min -1 .Results The linear range of polysorbate 80 was 418.80 ~1 256.40μg·mL -1 (r =0.999 3),and the average recovery was 98.55%,with the RSD of 0.99%.The linear range of EDTA was 100.56 ~301.68 μg·mL -1 (r =0.999 9),and the average recovery was 100.13%,with the RSD of 0.52%.Conclusion The method was rapid,accurate and reproducible.It can be used for the quality control of polysorbate 80 and EDTA in Fosaprepitant Dimeglumine for Injection.