摘要
建立了一种高效液相色谱法测定高哌嗪溴盐的新方法,确定了最优的色谱条件,色谱柱采用岛津VP-ODS色谱柱,柱长为250 mm,内径为4.6 mm;流动性采用V(甲醇)∶V(水)=10∶90(水相含30 mmol/L磷酸二氢钾,稀酸调p H=3.5);检测波长为220 nm;流速为1.0 m L/min;进样量为2.0μL。该分析方法填补了国内空白,分离度R≥1.5,线性相关系数达到了0.999以上,标准偏差均小于1.4%,加标回收率在98%~103%之间。实验结果表明,该方法能够满足工艺中控分析的需要。
A new method for determination of high piperazine bromine salt based on high performance liquid chromatography （HPLC） is developed. The optimal operation parameters are shown as follows ： VP-ODS chromatographic column ,250 mm of column length with 4. 6 mm of inner diameter, mixture of methanol and water （90/10） （water phase containing 30 mmol/L of potassium dihydrogen phosphate, pH = 3.5 ） as mobile phase ,220 nm of detection wavelength, 1.0 mL/min of the flow rate and 2. 0 p^L of sample. The separation degree of this method is no less than 1.5. The linear correlation coefficient is above 0. 999 with the standard deviation less than 1.4%. The recovery of standard addition is between 98% and 103%. It indicates that the new method can meet the needs of the centurial control analysis.
出处
《现代化工》
CAS
CSCD
北大核心
2015年第8期185-186,188,共3页
Modern Chemical Industry
基金
山东省政府"泰山学者"建设工程资金项目(ts20130918)
关键词
高哌嗪溴盐
高哌嗪
液相色谱
homopiperazine bromine salt
homopiperazine
performance liquid chromatography （HPLC）
