对甲基苯磺酰氯柱前衍生法测定水中哌嗪  

Determination of piperazine in water using pre-column derivatization with P-tosyl chloride

作　　者：李欣[1] 沈敏雅[1] 杨倩[1] 蔡天明[1] 

机构地区：[1]南京农业大学资源与环境科学学院,南京210095

出　　处：《分析试验室》2012年第12期48-52,共5页Chinese Journal of Analysis Laboratory

基　　金：江苏省省级环保科技项目(201005)资助

摘　　要：建立了一种高效液相柱前衍生化测定水中哌嗪含量的方法。选取对甲基苯磺酰氯(p-TSC)为衍生试剂对哌嗪进行衍生化,衍生产物利用液质联用(LC-MS)技术定性,高效液相色谱定量分析。方法采用Ultimate XB-C18色谱柱,以甲醇-水(体积比60:40)为流动相,流速为0.8 mL/min,检测波长为240 nm,室温下检测。实验结果表明,哌嗪的衍生化产物与过量衍生化试剂分离良好,在10～100 mg/L的范围内,哌嗪的浓度与其衍生产物峰面积呈现良好的线性关系,相关系数r>0.999。方法的检出限为0.09 mg/L,定量限为0.30 mg/L。回收率范围为88.2%～99.2%,相对标准偏差为2.5%～5.3%。通过正交反应试验确定了最佳衍生化条件:衍生温度为55℃,缓冲液pH为10.0,衍生时间10 min。A simple pre-column derivatization-high performance liquid chromatographic（HPLC） method with p-tosyl chloride as a derivative agent was established for the determination of anhydrous piperazine in water.After addition of p-tosyl chloride as the derivative agent,piperazine was derivatized.The derivatives were analyzed for qualitation and quantitation using LC-MS and HPLC,respectively.Separation was achieved at ambient temperature using an ultimate XB-C18 column,and isocratic elution with methanol–water（60：40,V/V） at a flow rate of 0.8 mL/min.The UV detection wavelength was 240 nm.Results showed that p-TSC and the piperazine derivatives were separated well and the correlation coefficient（r） of piperazine derivative with a linear range of 10~100 mg/L was over 0.999.The limits of detection and quantification were 0.09 mg/L and 0.30 mg/L,respectively.The average recoveries of piperazine were in the range of 88.2%~99.2% with the relative standard deviations（RSDs） of 2.5%~5.3%.Moreover,the results of orthogonal experiment revealed that the optimum conditions of derivatization reaction were： reaction temperature of 55 ℃,buffer of pH 10 and reaction time of 10 min.

关 键 词：哌嗪 对甲基苯磺酰氯 衍生化 高效液相 质谱 

分 类 号：O657.63[理学—分析化学]