反相离子对HPLC法测定盐酸二甲双胍中双氰胺的含量

目的建立反相离子对HPLC法测定盐酸二甲双胍中双氰胺含量的方法。方法采用Agilent HC-C18(2)色谱柱(250 mm×4.6 mm,5μm),以甲醇-10 mmol/L庚烷磺酸钠溶液(含0.8%三乙胺,用H3PO4调pH 3.0)(15∶85)为流动相;流速:1.0 mL/min;检测波长:218 nm;柱温:30℃。结果反相离子对HPLC法测定盐酸二甲双胍中双氰胺含量的线性范围为0.01~26.12μg/mL;相关系数r=0.999 9;重复性的RSD为1.8%;精密度RSD为1.6%;高、中、低3种浓度的加样回收率分别为98.8%,102.1%,103.6%;RSD分别为0.8%,1.2%,0.9%。结论此法简便、快速、准确、专属性好。

Determination of dicyandiamide in metformin hydrochloride by RP Ion-pair HPLC

Purpose To establish a RP Ion-pair HPLC method for the determination of dicyandiamide in metformin hydrochloride.Methods The separation was performed on an Agilent HC-C18(2)column(250 mm×4.6 mm,5 μm).The mobile phase was composed of methanol-10 mmol/L solution of heptane sulfonic acid sodium(including 0.8% triethylamine,adjusted to pH 3.0 with phosphoric acid)(15∶85).The flow rate was 1.0 mL/min.The detection was carried out with a UV detector at 218 nm.Column temperature was 30 ℃.Results The calibration curve of dicyandiamide was linear between 0.01 and 26.12 μg/mL.Correlation coefficient was 0.999 9.Repeatability of RSD was 1.8%.Accuracy of RSD was 1.6%.The quality control standard was reliable with a recovery rate of 98.8%,102.1% and 103.6%,RSD of 0.8%,1.2% and 0.9% for the solutions of the high,medium and low concentration of respectively.Conclusion This method is simple,rapid and accurate.It is suitable for the determination of dicyandiamide in metformin hydrochloride.