衍生化-气相色谱-质谱法测定染整助剂中的乙二胺四乙酸盐和二乙烯三胺五乙酸盐  

Determination of EDTA and DTPA in dyeing and finishing auxiliaries with derivatization-gas chromatography-mass spectrometry

作　　者：汤娟[1] 郑凯[2,3] 周佳[1] 石睿[1] 丁友超[1] 

机构地区：[1]江苏出入境检验检疫局工业产品检测中心,南京210001 [2]苏州大学纺织与服装工程学院,苏州215006 [3]张家港出入境检验检疫局,张家港215600

出　　处：《分析试验室》2016年第9期1019-1023,共5页Chinese Journal of Analysis Laboratory

基　　金：国家质量监督检验检疫总局科研项目(2015IK152);江苏省333工程科研项目资助计划项目(BRA2015468)资助

摘　　要：建立了乙二胺四乙酸盐（EDTA）和二乙烯三胺五乙酸盐（DTPA）衍生化成乙基酯的前处理方法以及气相色谱-质谱法测定乙基酯的方法。样品经甲酸酸化后,与乙醇发生酯化反应生成乙基酯,由正己烷提取,选择离子模式下由优化好的气相色谱-质谱进行定性定量分析。EDTA和DTPA质量浓度分别在0.2~20.0 mg/L和0.5~50.0 mg/L范围内线性关系良好,相关系数均不小于0.9991,两种不同阴性样品的3个不同浓度添加水平的平均回收率在91.6%~94.9%之间,相对标准偏差均不大于5.2%,EDTA和DTPA检出限分别为0.0609 mg/kg和0.145 mg/kg,定量限分别为0.194 mg/kg和0.476 mg/kg。方法能够满足染整助剂中EDT A和DT PA定性确证和准确定量的要求。A method of treating EDTA and DTPA into ethyl ester and determining with gas chromatography-mass spectrometry（GC-MS） was developed. Sample was acidified with formic acid and esterified with ethanol,after extracting by hexane. The qualitative and quantitative analysis was performed by the optimized GC-MS under selective ion mode. The calibration curves showed good linearity in the concentration range of 0. 2 ~ 20. 0 mg/L and 0. 5 ~ 50. 0 mg/L for the EDTA and DTPA with correlation coefficients not less than 0. 9991. The average recoveries of EDTA and DTPA for spiked samples at three different concentration levels in two different negative samples ranged from 91. 6% to 94. 9 %,with relative standard deviation（RSDs） not more than 5. 2 %. The limits of detection of EDTA and DTPA were 0. 0609 mg/kg and 0. 145 mg/kg,and the limits of quantitation were0. 194 mg/kg and 0. 476 mg/kg. The established method is reliable,accurate and sensitive,which is suitable for the determination of EDTA and DTPA in dyeing and finishing auxiliaries.

关 键 词：染整助剂 乙二胺四乙酸盐(EDTA) 二乙烯三胺五乙酸盐(DTPA) 气相色谱-质谱法 酯化反应 

分 类 号：TQ075[化学工程]