TSK-GEL色谱柱测定注射用氟氯西林钠聚合物的研究

Study on the determination of the polymer in flucloxacillin sodium for injection by TSK-GEL chromatographic column

目的:建立以TSK-GEL色谱柱测定注射用氟氯西林钠聚合物的方法,并进行方法适用性试验。方法:用球状蛋白色谱以亲水硅胶(分子量适用范围为1 000~10 000)为填充剂,TSK-GEL柱(300 mm×7.8 mm,5 μm);以磷酸盐缓冲液(pH 7.0)[0.04 mol/L磷酸氢二钠溶液-0.04 mol/L磷酸二氢钠溶液(61∶39)]-乙腈(95∶5)为流动相,流速为0.8 ml/min,检测波长为215 nm。结果:氟氯西林主峰能与其相邻聚合物峰达到有效分离。对照品溶液的线性范围为 0.195 9~ 97.970 8 μg/ml时,溶液浓度与聚合物峰的峰面积呈良好的线性关系(r =1.000 0),最低检测浓度为0.049 μg/ml 。结论:该方法可以准确、快速、高效地测定注射用氟氯西林钠中的聚合物含量,专属性强,重复性好。

Objective: To determine polymer content in Flucloxacillin Sodium for Injection, TSK-GEL chromatographic column method was established and the applicability of the method was also tested. Methods: Globular protein chromatographic grade hydrophilic silica was used as packing material (molecular weight range of 1 000 to 10 000). Chromatography conditions were as following: TSK-GEL column (300 mm×7.8 mm,5 μm);mobile phase was phosphate buffer(pH 7.0)[0.04 mol/L two sodium hydrogen phosphate solution-0.04 mol/L sodium dihydrogen phosphate(61∶39)]- acetonitrile (95∶5);flow rate was 0.8 ml/min, and detection wavelength was 215 nm. Results: The main peak of flucloxacillin can be effectively separated from its adjacent polymer peaks. The linear range of the reference solution was 0.195 9~97.970 8 μg/ml, and the concentration of the solution showed a great linear relationship with the peak area of the polymer ( r =1.000 0).The minimum detection concentration was 0.049 μg/ml, and the sensitivity test solution concentration was 0.2 μg/ml. Conclusion: The method is accurate, rapid and efficient for the determination of polymer content in Flucloxacillin Sodium for Injection.