反相离子对HPLC法同时测定盐酸二甲双胍中双氰胺和三聚氰胺的含量

Determination of Cyanoguanidine and Melamine in Metformin Hydrochloride by RP Ion-Pair HPLC

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 reverse phase ion-pair HPLC procedure for the quantification of cyanoguanidine and melamine in metformin hydrochloride is developed. A hypersil ODS Cl8 column （5 μm, 250 ×4.6 mm） is used with the mobile phase of acetoffitrile-ion-pair reagent solution （ 10 mmol/L sodium pentanesulfonate ＋ 10 mmol/L citric acid, pH = 3.0,10： 90） , With the flow rate 1.0 mL/min. The detection is carried out with a UV detector at wavelength of 217 nm. The results show that there is a good linear relationship in the concentration range of 0.02 - 20 μg/mL for cyanoguanidine （ R = 0. 999 9） and 0.02 - 50 p^g/mL for melamine （ R = 0. 999 9 ）. The average recovery is 97.6% with RSD of 0.29% for cyanoguanidine, and 96.5% with RSD of 0.32% for melamine. The detection limits are 4.0 ng/mL for eyanoguanidine, and 6.0 ng/mL for melamine, respectively. The method is rapid and simple, accurate and sensitive. It can be used to test the related substances in metformin hydrochloride.