盐酸二甲双胍肠溶胶囊中二甲胺残留量的测定

目的:建立盐酸二甲双胍肠溶胶囊中二甲胺残留量的柱前衍生HPLC测定方法.方法:用十八烷基硅烷键合硅胶为填充剂,以1.0%甲酸溶液-乙腈为流动相,采用梯度洗脱程序,检测波长为265 nm.结果:在选定的色谱条件下,二甲胺在0.254~4.065μg·mL-1的浓度范围内线性关系良好(r>0.999);精密度试验的RSD为1.6%,稳定性试验的RSD为1.5%;回收率为100.3%(n=9,RSD<1.5%).二甲胺的检测限为0.0508μg·mL-1,在测定的3批样品中,3批均检出二甲胺分别为0.01%,0.04%,0.02%.结论:本方法专属性强,准确度高,重现性好,能控制盐酸二甲双胍肠溶胶囊中二甲胺残留量.

Determination of Residual Dimethylamine in Metformin Hydrochloride Enteric-coated Capsules

Objective:To establish pre-column derivatization and HPLC method for the determination of dimethylamine in Metforminhydrochloride enteric-coated capsules.Methods:With octadecylsilane chemically bonded silica as filler,With 1.0%formic acid solution(A)and acetonitrile(B)as mobile phase,ingradientelution,and the detectionwavelength was 265 nm.Results:In the spectrum of the selectedconditions,A good linearity observed in the range of 0.254~4.065μg·mL-1(r>0.999)dimethylamine.The RSD of the precision was 1.6%,The RSD of stability test was 1.5%;The recovery was 100.3%(n=9,RSD<1.5%).The limit of detection was 0.0508μg·mL-1.The test results of 3 batches of samples was 0.01%,0.04%,0.02%.Conclusion:The method is specific,accurate and reproducible for the determination of dimethylamine in metformin hydrochloride enterin-coated capsules.