离子交换HPLC法测定唑来膦酸的含量及有关物质

Determination of zoledronic acid and its related substances by ion exchange HPLC

目的采用阴离子交换高效液相色谱法测定唑来膦酸的含量及有关物质。方法HypersilSAX强碱型阴离子交换色谱柱(250mm×4.6mm,5μm),以0.03mol/L焦磷酸钠溶液-甲醇(85∶15)(混合后磷酸调pH为7.0)为流动相,流速约1ml/min,检测波长210nm,室温。结果唑来膦酸与有关物质分离良好,唑来膦酸在0.8～200μg/ml的浓度范围内,浓度与峰面积呈很好的线性关系(r=0.99999),平均回收率为99.78%,RSD=0.43%(n=9),最低检测浓度为0.04μg/ml。结论该方法分离效果好,准确、可靠、精密。

Objective To establish an ion-exchange HPLC method for the determination of zoledronic acid and its related substances. Methods The chromatographic column was Hypersil SAX (250mm×4.6mm, 5μm); with 0.03mol/L sodium pyrophosphate-methanol (adjust to pH7.0 with phosphoric acid) (85∶15) as the mobile phase; the flow rate was 1.0ml/min, the detection wavelength was set at 210nm and the column temperature maintained at room temperature. Results The calibration curve was linear in the concentration range of 0.8～200μg/ml (r=0.9999). The average recovery rate was 99.87% and RSD 0.43% (n=9). The detection limits were 0.04μg/ml. Conclusion The method is accurate, sensitive and reproducible.