盐酸头孢吡肟中高分子聚合物含量测定方法学研究

Study on the determination of high molecular polymers in cefepime hydrochloride

目的采用高效液相色谱法测定盐酸头孢吡肟中高分子聚合物,并进行方法学研究。方法采用分子排阻色谱法,色谱柱:Sephadex G-10柱(13.0 mm×400 mm,TIANHE);流动相:流动相A为pH7.0的0.01mol/L磷酸盐缓冲液[0.01 mol/L Na2 HPO4溶液-0.01 mol/L NaH2 PO4溶液(体积比61∶39)],流动相B为水;流速:1.0 mL/min;检测波长:254 nm;进样量:100μL;以头孢噻肟作为对照品加校正因子外标法定量[Mr(头孢吡肟)/Mr(头孢噻肟)=1.055]。结果头孢吡肟在0.88～51.70 mg/mL范围内与盐酸头孢吡肟高分子聚合物峰面积呈良好的线性关系(r=0.999 7);头孢噻肟在58.55～136.61μg/mL范围内与头孢噻肟缔合物的峰面积呈良好的线性关系(r=0.999 8)。检测限为2.7×10-3μg,定量限为5.4×10-3μg。结论该方法能较好地分离盐酸头孢吡肟及其高分子聚合物,可用于盐酸头孢吡肟中高分子聚合物的检查。

Objective To develop and validate the method of determining high molecular polymers in cefepime hydrochloride.Methods Molecular exclusion chromatography was performed with Sephadex G-10（13.0 mm×400 mm,TIANHE） gel column.The mobile phase A was 0.01 mol/L phosphate buffer（pH7.0） and the mobile phase B was water with a flow rate of 1.0 mL/min.The detection wavelength was 254 nm and the injection volume was 100 μL.The polymers was assayed by external standard method with a correct factor（the molecular weight of cefepime/the molecular weight of cefotaxime is 1.055）.Results The calibration curve of high molecular polymers in cefepime hydrochloride was linear within the range of 0.88-51.70 mg/mL（r=0.999 7）.And the calibration curve of associations in cefotaxime was linear within the range of 58.55-136.61 μg /mL（r=0.999 8）.The limit of detection was 2.7×10-3 μg and the limit of quantitation was 5.4×10-3 μg.Conclusion This method can be used to separate the polymers from cefepime hydrochloride and control the quality of cefepime hydrochloride and its preparations.