HPLC法测定氟氯西林钠颗粒中谷氨酸钠的含量

Assay of Glutamate Sodium in Fludoxacillin Sodium Granule by HPLC

建立快速直接测定氟氯西林钠颗粒中谷氨酸钠含量的HPLC法,提高分析效率和结果的可靠性。色谱柱选用强极性的Lichrospher Diol柱;流动相为0.01M磷酸二氢铵缓冲液(pH=2.0)-乙腈(15:85)为流动相;用pH 2.0磷酸二氢铵缓冲液-乙腈混合溶液(30:70)为溶剂。检测波长为206nm;谷氨酸钠在上述色谱条件下有合适的响应和保留,制剂中主药氟氯西林钠和所有辅料均随溶剂峰提前洗脱,与谷氨酸钠主峰实现了良好分离;当进样体积为50μl时,谷氨酸钠在0.0051～0.5072mg·ml^(-1)浓度范围内与峰面积有良好的线性关系,r=0.9998(n=10);方法的准确性、重复性和专属性均令人满意。

A HPLC method has been established for the determination of glutamate sodium in flucloxacillin sodium granule. The separation was performed on a Lichrospher Diol column (250mm × 4.6mm, 5μm). The mobile phase composed of 0.01mol·L-1 NH4H2PO4 buffer solution (pH 2.0) - acetonitrile (15:85). The solvent used to prepare standard solution and test solution was the mixture of 0.01mol·L-1 NH4H2PO4 buffer solution (pH 2 '0) - acetonitrile (30:70). The detection was carried out on a UV detector at 206nm. The flow rate was 1.0ml·min-1. When the injection volume was 50μl, the standard curves of glutamate was linear in the range of 0.0051 - 0.5072mg·ml-1 (r = 0.9998, n = 10). The RSD for repetition was 1.1% and the average recovery was 96.9% (RSD = 1.3% , n = 9). This method offered a rapi, repeatable and accurate procedure suitable for assay of glutamate sodium in flucloxacillin granule.