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建立一种简单的反相离子对HPLC方法测定盐酸二甲双胍中的双氰胺和三聚氰胺的含量.使用Hypersil ODS C18反相色谱柱(5μm;250×4.6 mm),乙腈-离子对试剂水溶液(10 mmol/L戊烷磺酸钠+10 mmol/L柠檬酸,pH为3.0,体积比10∶90)为流动相,流速1.0 mL/min,检测波长217 nm,柱温25℃.结果表明:双氰胺在0.02~20μg/mL浓度范围内线性关系良好,相关系数R=0.999 9,平均回收率为97.6%,RSD=0.29%;三聚氰胺在0.02~50μg/mL浓度范围内线性关系良好,相关系数R=0.999 9,平均回收率96.5%,RSD=0.32%.双氰胺和三聚氰胺的检出限分别为4.0 ng/mL和6.0 ng/mL.该方法简单、快速、准确、灵敏,适于同时测定盐酸二甲双胍制剂中的双氰胺和三聚氰胺的含量.
A simple reversed-phase ion-pair HPLC method was developed for the determination of dicyandiamide and melamine in metformin hydrochloride.Hypersil ODS C18 reversed-phase column (5 μm; 250 × 4.6 mm), acetonitrile-ion pair reagent solution / L sodium pentane sulfonate + 10 mmol / L citric acid, pH 3.0, volume ratio 10:90) as the mobile phase at a flow rate of 1.0 mL / min with a detection wavelength of 217 nm and a column temperature of 25 ° C. The results showed that: The linearity was good in the range of 0.02 ~ 20μg / mL with the correlation coefficient R = 0.999 9, the average recovery 97.6% and RSD 0.29%. The linearity of melamine in the range of 0.02 ~ 50μg / mL was good. The correlation coefficient R = 0.999 9, the average recovery was 96.5% and the RSD was 0.32% .The detection limits of dicyandiamide and melamine were 4.0 ng / mL and 6.0 ng / mL, respectively.The method was simple, rapid, accurate and sensitive and suitable for simultaneous determination Dicyandiamide and melamine in metformin hydrochloride formulations.