邻苯二甲醛衍生法测定水中二乙烯三胺  

Determination of diethylenetriamine in water with precolumn O-phthalaldehyde derivation

作　　者：刘汉方[1] 马德库[1] 梁戈清[1] 刘广舒[1] 

机构地区：[1]中国石油天然气集团公司石油职业卫生技术服务中心中心实验室,河北廊坊065000

出　　处：《中国卫生检验杂志》2013年第10期2227-2229,共3页Chinese Journal of Health Laboratory Technology

基　　金：2011年廊坊市科研课题(市级)项目(2011013022)

摘　　要：目的建立高效液相荧光检测器法测定水质中二乙烯三胺的方法。方法样品与邻苯二甲醛衍生剂混合后,100℃水浴5 min,衍生产物使用ODS柱,甲醇+乙酸钾水溶液(55+45)作为流动相,流速1.0 ml/min,激发波长351 nm,发射波长411 nm,荧光检测器测定。结果二乙烯三胺在0.05 mg/L～10 mg/L范围内呈现良好的线性,浓度与吸光度相关系数r=0.9995,最低检出浓度为0.015 mg/L,回收率在98%～103%之间,变异系数小于3%。结论本法测定二乙烯三胺操作简便,结果准确可靠,可以满足水质中二乙烯三胺测定要求。Objective To establish a high performance liquid chromatography （HPLC）with fluorescence detection method for the determination of diethylenetriamine in water. Methods The sample was mixed with O - phthalalde- hyde （OPA）in 100 ℃ water bath for 5 rain. Then the derivatives were separated on an CDS column using the mo- bile phase consisting of methyl alcohol ＋ potassium acetate solution（55 ＋ 45 ） , and the flow rate was 1.0 ml/min. Finally, the derivative sample was detected by fluorescence detector with excitation wavelength （hex） at 35 lnm and emission wavelength （hem） at 411 nm. Results The calibration curve was linear within the range of 0.05 mg/L 10.0 mg/L. The correlation coefficient was 0. 9995. The detection limit was 0. 015 mg/L and the recoveries were 98% - 103% , with relative standard deviations of 3%. Conclusion This method is simple, convenient, accurate and reliable, so it is suitable for determination of diethylnetriamine in water.

关 键 词：邻苯二甲醛 液相色谱 二乙烯三胺 荧光检测器 

分 类 号：O657.72[理学—分析化学]