离子色谱法测定盐酸二甲双胍药物中二甲胺的含量

Determination of dimethylamine in metformin hydrochloride by ion chromatography

目的建立离子色谱法测定盐酸二甲双胍药物中二甲胺的含量。方法采用阳离子交换柱Dionex IonPac CS12A(4 mm×250 mm),以甲磺酸溶液为淋洗液进行梯度洗脱,流速1.0 mL·min^(-1),柱温30℃,进样体积25μL,采用抑制型电导器检测。结果原料、胶囊及片剂中的二甲胺在0.050~50μg·mL^(-1)与峰面积线性关系良好(r=1.000),定量限和检测限分别为6 ng·mL^(-1)和2 ng·mL^(-1)。缓释片中的二甲胺在0.025~5.0μg·mL^(-1)与峰面积线性关系良好(r=0.9990),定量限和检测限分别为6 ng·mL^(-1)和3 ng·mL^(-1)。原料及制剂中二甲胺的回收率在92.5%~103.5%,RSD<4.0%。结论该方法操作简便,准确可靠,可用于盐酸二甲双胍药物中二甲胺含量的检测。

Objective To determine the dimethylamine(DMA)in metformin hydrochloride by ion chromatography method.Methods The determination was conducted on a Dionex IonPac CS12A(4 mm×250 mm)column and a protective column[Dionex IonPac CG12A(4 mm×50 mm)]with methanesulfonic acid solution as the eluent.The flow rate was 1.0 mL·min^(-1).The column temperature was 30℃,and the injection volume was 25μL.Results In non-sustained released dosage forms,the method showed good linearity at 0.050~50μg·mL^(-1)(r=1.000)for DMA,the limit of quantification and detection were 6 ng·mL^(-1) and 2 ng·mL^(-1),respectively.In sustained released dosage forms,the method showed good linearity at 0.025~5.0μg·mL^(-1)(r=0.9990)for DMA,the limit of quantification and detection were 6 ng·mL^(-1) and 3 ng·mL^(-1),respectively.The recoveries of raw materials and its preparations ranged from 92.5%to 103.5%with the RSD less than 4.0%.Conclusion The method is simple,accurate and reliable for the determination of DMA in metformin hydrochloride and its preparations.