TSK凝胶色谱系统测定头孢呋辛酯片的高分子聚合物

Determination of the high molecular polymers in cefuroxime axetil tablets by TSK-gel chromatography system

目的建立TSK凝胶色谱系统测定头孢呋辛酯片中高分子聚合物的方法。方法采用HPLC法,色谱柱为TSK-gel G2000 SWXL(7.8 mm×300 mm),以水-甲醇(10∶90,V/V)为流动相,流速为0.5 ml/min,检测波长为278 nm,进样体积为20μl。结果高分子聚合物峰与头孢呋辛酯峰能有效分离,辅料无干扰,头孢呋辛酯主成分的线性范围为10.44μg/ml^1 471.37μg/ml(r=0.999 8);供试品溶液的浓度为0.312 mg/ml^1.561 mg/ml时,与聚合物峰面积呈良好线性关系(r=0.999 8);检出限为3.13μg/ml,定量限为10.44μg/ml;方法的精密度良好(RSD=0.15%);样品测定的重复性(RSD=0.51%)与重现性较好(RSD=0);供试品溶液室温放置不稳定,故需临用新制,配制后低温放置。结论该方法简便、快速、灵敏度高、重现性好,克服了传统聚合物检测方法分析时间长,无法检测脂溶性样品的缺点。可用于头孢呋辛酯片及其他脂溶性抗生素中高分子聚合物的检测。

Objective To establish a method for the determination of high molecular polymers in cefuroxime axetil tablets by TSK - gel chromatography system. Methods The detection was conducted under the following conditions by high - pressure liquid chromatography（HPLC） ： Chromatographic column was TSK -gel G2000 SWXL （7.8 mm x 300 ram） ; the mobile phase was water - methanol（ 10：90, V/V） ; the flow rate was 0.5 ml/min; the detection wavelength was 278 nm and the injection vol- ume was 20 μ1. Results High molecular polymers was separated completely from cefuroxime axetil. The accessories made no interference. The linear of cefuroxime axeti] was within 10.44 μg/ml - 1 471.37 μg/ml（ r =0. 999 8）. When the linear range of the polymers examined was within 0. 312 mg/ml - 1. 561 mg/ml（ r =0. 999 8） , good linearity was obtained with the peak ar- ea of polymers. The limit of detection was 3.13 μg/ml, the limit of quantification was 10.44 μg/ml. The specificity was good （RSD = 0. 15 % ）, the repetitiveness （RSD = 0.51% ） and the reproducibility（RSD = 0） were fine. The sample solution was nut stable at room temperature, so it should be prepared just before using, and kept in low temperature. Conclusion The method is simple, rapid, sensitive and reproducible, which overcomes the shortcomings of the traditional polymer detection method for long time and can not deteet the fat soluble sample. It＇s suitable for the determination of the high molecular polymers in cefu- roxime axetil tablets and other liposolubile antibiotics.