抑制电导-离子色谱法测定羧甲基壳聚糖中二甘醇酸

Determination of Diglycolic Acid Remained in Carboxymethyl-Chitosan by Suppression Conductivity-Ion Chromatography

建立了抑制电导—离子色谱法用于直接测定手术用羧甲基壳聚糖中残留二甘醇酸。对比分析了3种不同离子交换色谱柱,结果表明:Shodex IC SI-524E阴离子分析柱性能最优。采用该分离柱,比较了不同的淋洗液浓度,最终选择8 mmol/L的碳酸钠溶液为淋洗液。在确定的分离和洗脱条件下,该方法以20μL进样量对二甘醇酸的检出限为1.98μg/L,完全满足医药行业标准规范的要求,测定羧甲基壳聚糖样品中残留二甘醇酸的精密度(RSD=2.30%(n=7))和回收率(95.33%)也满足实际样品分析的要求。测试过程在15 min内可以完成,证明抑制电导—离子色谱法是测定羧甲基壳聚糖中残留二甘醇酸的一种简便、快速、准确的方法。

An ion chromatography method with suppressed conductivity detector was developed for the determination of diglycolic acid remained in Surgical Carboxymethyl-Chitosan.3 kinds of anion-exchange columns were studied and the Shodex IC SI-524E column was selected for best resolution.Then concentrations of sodium carbonate eluent were compared,and the 8 mmol/L one was used at the following experiments.The results showed that the ion chromatography method completely satisfied the requirement of medicine industry standard with a determination limit of 1.98μg/L by 20μL as sample injection volume.Also a RSD of 2.30%(n=7)of the peak area,a recovery ratio of 95.33 and a whole analysis process within 15mins proved a handy,fast,veracious and practical method for diglycolic acid remained in surgical Carboxymethyl-Chitosan.