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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
【摘要】 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。
【Abstract】 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 IonPacAS11 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 calibration 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 CMC-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.
- 【文献出处】 药物分析杂志 ,Chinese Journal of Pharmaceutical Analysis , 编辑部邮箱 ,2009年09期
- 【分类号】R927
- 【被引频次】3
- 【下载频次】268