高效液相色谱法测定亚甲基二磷酸含量

Determination of Medronic Acid by Reversed-Phase High-Performance Liquid Chromatography

采用反相高效液相色谱法/蒸发光散射检测器(ELSD)研究了亚甲基二磷酸含量测定及相关物质的分析方法。以Symmetry C8为固定相,V(30mmol/L正戊胺(用乙酸调节pH 5.0))∶V(甲醇)=98∶2为流动相,流速为1mL/min,蒸发光散射检测器检测亚甲基二磷酸对照品溶液。在该条件下,亚甲基二磷酸及相关物质(包括合成过程中残留的亚磷酸及氧化分解产物磷酸)的分离良好。方法的线性范围在600～4 000mg/L,线性回归方程为:lgA=1.943 6lgC+16.212,r=0.999 6,检出限为200mg/L,回收率在98%～102%,适用于亚甲基二磷酸原料的常规检测及有关物质的检查。

An isocratic liquid chromatographic method with evaporative light scattering detection（ELSD） was developed for the determination of medronic acid and its related substances.Volatile pentylamine was used as the ion-pairing agent.Separations were performend on a Symmetry C8 column with an mobile phase of 98∶2（V∶V） 30 mmol/L pentylamine（pH 5.0,adjusted with acetic acid）-methanol.The mobile phase was delivered at a flow-rate 1.0 mL/min.The method is applicable to the routine analysis and the quality control of medronic acid.