高效分子排阻色谱法测定头孢羟氨苄胶囊中的高分子杂质

Determination of High Molecular Weight Impurities in Cefadroxil Capsules by HPSEC

目的建立高效分子排阻色谱(HPSEC)法测定头孢羟氨苄胶囊中的高分子杂质。方法采用TSK-GEL G2000SWXL凝胶色谱柱(30 cm×7.8 mm×5μm);流动相:0.005 mol.L-1醋酸铵溶液(用稀氨溶液调节pH值至7.0);流速:0.7 mL.min-1;检测波长:263 nm。结果高分子杂质在头孢羟氨苄质量浓度0.035～5.00 mg.mL内线性关系良好(r=0.999 9);头孢羟氨苄的检测限为1.5 ng,高分子杂质的定量限以头孢羟氨苄计为4.9 ng;对照溶液重复进样(n=6)的精密度(RSD)为0.24%,样品测定(n=6)的重复性(RSD)为1.35%。结论本方法操作简单,专属性强,灵敏度高。

OBJECTIVE To establish a high performance size exclusion chromatography（HPSEC） method for the determination of high molecular weight impurities in cefadroxil capsules.METHODS A TSK-GEL G2000S WXL column（30 cm×7.8 mm×5 μm） was used with the mobile phase consisting of 0.005 mol·L-1 ammonium acetate solution（adjust to pH of 7.0 with diluted ammonia solution） at a flow rate of 0.7 mL·min-1,and the detection wavelength was 263 nm.RESULTS The calibration curves for high molecular weight impurities were linear in the range of 0.035-5.00 mg·mL of cefadroxil（r=0.999 9）.The limit of detection for cefadroxil was 1.5 ng,and the limit of quantitation for high molecular weight impurities calculated as cefadroxil was 4.9 ng.The RSD for replicate injections of reference solution（n=6） was 0.24%,and the repeatability for 6 measurements was 1.35%.CONCLUSION The HPSEC method is simple,specific and sensitive.