克拉维酸钾及主要原料中大分子蛋白杂质的测定

Determination of macromolecular protein impurities in potassium clavulanate and its major raw material

建立了凝胶排阻色谱对克拉维酸钾及其原料克拉维酸叔辛胺中的残余蛋白进行检测的方法。采用TSK gel G3000 SWXL凝胶色谱柱(5μm,7.8×300 mm),流动相为磷酸盐缓冲溶液,流速为0.8 m L/min,紫外检测波长为220 nm。对照品牛血清白蛋白(BSA)在0.249~49.9μg/m L内线性关系良好(R2=0.9997),平均回收率为101.2%,RSD为0.7%,检测限为0.05μg/m L。方法为同类药物中的大分子蛋白检测提供了有效手段。

A gel exclusion chromatography method was established for the determination of the residual protein in potassium clavulanate and its raw material tert-octylammonium clavulanate. A TSK gel G3000 SWXL column（ 5 μm,7. 8 × 300 mm） was used with the mobile phase consisted of phosphate buffer solution at a flow rate of 0. 8 m L/min with the detection wavelength and at 220 nm. The linear range of BSA was 0. 249 ～ 49. 9 μg/m L（ R2= 0. 9997）,The average recovery was 101. 2% and RSD was 0. 7% and the lowest limit of detection was 0. 05 μg/m L. The proposed method was proven to be simple,accurate and sensitive. This study provided a new approach for the analysis of residual protein in other similar drugs.