高效液相色谱法同时测定高哌嗪反应液中的两步中间体

Simultaneous determination of two steps intermediates of homopiperazine by high performance liquid chromatography

建立了同时测定高哌嗪反应液中的两步中间体含量的高效液相色谱方法,实现了对高哌嗪合成工艺中控分析的目标。采用Shimadzu高效液相色谱仪和VP-ODS C18色谱柱,以V(乙腈)∶V(25 mmol/L磷酸二氢钾)=1∶1(以稀磷酸调节pH为3.5)为流动相。在流速为1.0 mL/min,紫外吸收波长为236 nm条件下,两步中间体线性相关系数均达到0.999以上,标准偏差均小于2.0%,加标回收率在97%～103%之间。实验结果表明,该方法能够满足该工艺的中控分析的要求。

A HPLC method is developed for the simultaneous determination of two steps intermediates of homopiperazine, which achieves the objective of middle-controlled analysis. A Shimadzu high performance liquid chromatograph and a VP-ODS C18 column are used for the separation. The mixture of CAN and water （including 25 mmol/L potassium dihydrogen phosphate, adjusting pH to 3.5 with phosphoric acid） = 1： 1 （V/V） is used as the mobile phase. At a flow rate of 1.0 mL/min, the correlation coefficients of the intermediates are both above 0. 999, which are determined by an ultraviolet absorbance detector at 236 nm. Under these conditions, the relative standard deviations are both less than 2. 0% and the spiked recoveries are 97% - 103%. The experiment results show that this method can reach the requirement of the middle-controlled analysis.