摘要
目的:建立高效分子排阻色谱(HPSEC)法测定头孢尼西钠中的聚合物,并与葡聚糖凝胶G^(-1)0为填料的凝胶色谱法进行比较。方法:HPSEC法采用表面键合亲水薄膜硅胶为填料的色谱柱(Zenix SEC^(-1)50,7.8 mm×300 mm);流动相为0.01mol·L^(-1)磷酸盐缓冲液-乙腈(95∶5);流速:1.0mL·min^(-1);检测波长250 nm。结果:HPSEC法:头孢尼西及其聚合物分别在1~100μg·mL^(-1)和0.25~1.75 mg·mL^(-1)范围内的线性关系良好,头孢尼西的定量限为1.0ng·mL^(-1),精密度(RSD)为0.57%,聚合物测定重复性(RSD)为1.01%。凝胶色谱法:头孢尼西的定量限为500 ng·mL^(-1),精密度(RSD)为1.81%,聚合物测定重复性(RSD)为3.08%。HPSEC和凝胶色谱法测得的样品中头孢尼西聚合物的量分别为1.31%和0.23%。结论:HPSEC法适于测定头孢尼西钠聚合物,较凝胶色谱法专属性强,灵敏度高,重复性好,操作简便。
OBJECTIVE To establish a high performance size exclusion chromatography（HPSEC）method for determination of polymer in cefonicid sodium for injection and compare with gel chromatography by sephadex G^-10 column.METHODSA Zenix^-150 column（7.8 mm×300 mm）was used with mobile phase of 0.01 mol·L^-1 phosphate buffer solution（pH7.0）-acetonitrile（95∶5v/v）at a flow rate of 1.0mL·min^-1,and detection wavelength at 250 nm.RESULTS HPSEC：calibration curves were linear in range of 1-100μg·mL^-1 for cefonicid by reference solution（r=0.999 9）and quantification limit of cefonicid was 1.0ng·mL^-1.Calibration curves were linear in range of 0.25^-1.75 mg·mL^-1 for polymer by sample（r=0.999 5）.RSD for precision of cefonicid by reference solution was less than 0.57% and polymer by sample was less than 1.01%.Gel chromatography：quantification limit of cefonicid was 500 ng·mL^-1.RSD for precision of cefonicid by reference solution was less than 1.81% and polymer by sample was less than 3.08%.Mean amount of polymer from seven batches was 1.31% for HPSEC and 0.23%for gel chromatography.CONCLUSION HPSEC method is suitable for determination of polymer in cefonicid sodium for injection,and has superior specificity,sensitivity,precision,and is simpler than gel chromatography.
出处
《中国医院药学杂志》
CAS
CSCD
北大核心
2016年第23期2070-2073,共4页
Chinese Journal of Hospital Pharmacy
