同位素 ›› 2012, Vol. 25 ›› Issue (1): 33-36.DOI: 10.7538/tws.2012.25.01.0033

• 放射性药物与标记化合物 • 上一篇    下一篇

高效液相色谱法测定亚甲基二磷酸含量

赵秀岩;王晓静;付博;叶肇云;柳银黎   

  1. 原子高科股份有限公司,北京102413
  • 收稿日期:1900-01-01 修回日期:1900-01-01 出版日期:2012-02-20 发布日期:2012-02-20

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

ZHAO Xiu-yan;WANG Xiao-jing;FU Bo;YE Zhao-yun;LIU Yin-li   

  1. Beijing Atomic High Tech Co. Ltd., Beijing 102413, China
  • Received:1900-01-01 Revised:1900-01-01 Online:2012-02-20 Published:2012-02-20

摘要: 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(30 mmol/L正戊胺(用乙酸调节pH 5.0))∶V(甲醇)=98∶2为流动相,流速为1 mL/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600~4 000 mg/L,线性回归方程为:lgA=1.943 6 lgC+16.212,r=0.999 6,检出限为200 mg/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。

关键词: 亚甲基二膦酸, 高效液相色谱法, 蒸发光散射器

Abstract: 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.

Key words: medronic acid, reverse-phase HPLC, evaporative light-scattering detector