高效液相色谱法测定肌酸粉中一水肌酸、肌酸酐和双氰胺含量

Determination of creatine monohydrate,creatinine and dicyandiamide in creatine powder by high performance liquid chromatography

目的建立高效液相色谱法同时检测肌酸粉中一水肌酸、肌酸酐和双氰胺含量的分析方法。方法样品用水溶解稀释至一定溶度,过滤膜即得样品供试液。采用高效液相色谱法(high performance liquid chromatography,HPLC)测定,10 mmol/L磷酸二氢钠溶液(氨水调PH至10.5)作为流动相,检测波长为220 nm,流速0.8 mL/min,外标法定量。结果本方法在10 min内完成3种目标化合物的分离分析。试样中一水肌酸浓度在0.204~1.02 mg/mL的范围内线性关系良好,相关系数r>0.999。在三水平不同浓度一水肌酸标准品添加下,一水肌酸的回收率为100.3%。试样中肌酸酐浓度在0.530~6.36μg/mL的范围内线性关系良好,相关系数r>0.999。在三水平不同浓度肌酸酐标准品添加下,肌酸酐的回收率为99.0%。试样中双氰胺浓度在0.0531~0.637μg/mL的范围内线性关系良好,相关系数r>0.999。在三水平不同浓度双氰胺标准品添加下,双氰胺的回收率为106.1%。结论该方法快速、准确、灵敏,适合同时测定肌酸粉中一水肌酸,肌酸酐和双氰胺含量。

Objective To establish a method for simultaneous determination of creatine monohydrate,creatinine and dicyandiamide in creatine powder by high performance liquid chromatography. Methods The sample was dissolved and diluted with water to a certain solubility,and the sample solution was obtained by filtering the membrane. It was determined by high performance liquid chromatography(HPLC). The mobile phase was 10 mmol/L sodium dihydrogen phosphate solution(pH was adjusted by ammonia water to 10.5). The detection wavelength was 220 nm,the flow rate was 0.8 mL/min,and the external standard method was used for quantitative analysis. Results The separation and analysis of three target compounds were completed in 10 minutes. The linear relationship of creatine monohydrate was good in the range of 0.204-1.02 mg/mL,and the correlation coefficient(r) was greater than 0.999. The recovery rate of creatine monohydrate was 100.3% at three levels with different concentrations of creatine monohydrate standard. The linear relationship of creatinine concentration was good in the range of 0.530-6.36 μg/mL,and the correlation coefficient(r) was greater than 0.999. The recovery rate of creatinine was 99.0% at three levels with different concentrations of creatinine standard. The linear relationship of dicyandiamide was good in the range of 0.0531-0.637 μg/mL,and the correlation coefficient(r) was greater than 0.999. The recovery rate of dicyandiamide was 106.1% at three levels with different concentrations of dicyandiamide standard. Conclusion The proposed method is fast,accurate and sensitive,which is suitable for the simultaneous determination of creatine monohydrate,creatinine and dicyandiamide in creatine powder.