离子色谱法测定羧甲基淀粉钠中氯乙酸的残留量

Ion chromatography determination of chloroacetic acid in CMC-Na

目的:建立离子色谱法测定羧甲基淀粉钠中氯乙酸残留量。方法:采用离子色谱柱:IonPacAS11阴离子分离柱(4.0mm×250mm),AG-11保护柱(4.0mm×50mm);淋洗液为10mmol·L-1氢氧化钾溶液,流速1.0mL·min-1;电导检测器。结果:被测物氯乙酸和氯离子能得到很好的分离,空白对照无干扰;进样浓度在0.02～18.42μg·mL-1范围内与峰面积呈良好的线性关系(r=1.000);平均回收率为101.7%(n=9);最低检出限为0.15ng。结论:本试验建立的色谱方法灵敏、准确,适合药用辅料羧甲基淀粉钠原料中氯乙酸残留量的检测。

Objective： To establish a method of ion chromatography for determination of chloroacetic acid in sodium carboxymethyl starch（ CMC- Na）. Methods： An ion chromatography was developed, and an IonPacASll anion chromatography column （4.0 mm× 250 mm） with an AG - 11 guard column （4.0 mm × 50 mm） was adopted, with the eluent of 10 mmol · L-1 potassium hydroxide solution. The flow rate was 1.0 mL · min- 1, and the detector was conductivity detector. Results： Chloroacetic acid in CMC - Na and chloridion were separated completely. The cali- bration curve of chloroacetic acid showed a good linear relationship in the range of 0.02 -18.42 μg · mL-1 （r = 1. 000 ） ;The average recovery of chloroacetic acid in C MC -Na was 101.7% （n = 9）. The LOD of chloroacetic acid was 0.15 ng. Conclusion： The method is accurate, reliable,and can be used for the determination of residue of chloroacetic acid in CMC -Na and other pharmaceutical excipients.