反相高效液相色谱-荧光检测法测定粉针剂中帕米膦酸二钠含量及有关物质

Determination of Pamidronate disodium and its impurity in injection by HPLC with fluorescence detection

目的:建立帕米膦酸二钠粉针剂中含量及有关物质的检测方法。方法:采用反相高效液相色谱-荧光检测法,色谱柱为迪马DiamondC1(8250mm×4.6mm,5μm),流动相为乙腈:0.4%EDTA的氢氧化钠溶液(21:79),检测波长为395nm(激发波长)和480nm(发射波长),流速为1mL/min。结果:帕米膦酸二钠浓度线性范围为0.6μg/mL～16.0μg/mL,日内及日间精密度均小于3.7%,检出灵敏度(S/N=3)小于3.0ng,平均回收率为101.0%,有关物质β-丙氨酸检出限量小于0.02%。结论:本法简单、灵敏、快速,可用于帕米膦酸二钠粉针剂中含量及有关物质的测定。

Objective：To establish a simple method for determination of impurities and Pamidronate disodium amounts in injection.Methods：The high performance liquid chromatography with fluorescence detection was carried out with Diamond Cl8 （250mm×4.6mm,5μm）as separation column, aeetonitrile：0.4% EDTA NaOH solution （21：79） as mobile phase, Ex 395nm and Em 480nm as detector wavelength.Results：The linear range of Pamidronate disodium was over 0.6μg/mL--16.0μg/mL.The average recovery was 101.0% with precision of less than 3.7%.The detection limits was 3.0ng （S/N=3） for Pamidronate disodium, the relative min-imum detection amount was 0.02% for β-alanine impurity.Conclusion：The method was simple, sensitive, rapid and could be used for the quality control of Pamidronate disodium injection.