Fe^(3+)络合-离子对液相色谱-串联质谱测定纺织品中乙二胺四乙酸盐和二乙烯三胺五乙酸盐  

Determination of ethylenediaminetetraacetic acid(EDTA) and diethylenetriaminepentaacetic acid(DTPA) in textile by means of formation of their Fe^(3+) complex with ion-paired liquid chromatography-tandem mass spectrometry

作　　者：丁友超[1] 李建军[1] 吴丽娜[1] 曹锡忠[1] 钱凯[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

出　　处：《分析试验室》2012年第8期27-32,共6页Chinese Journal of Analysis Laboratory

基　　金：国家质量检验公益性行业科研专项项目(200910013);江苏检验检疫局科研课题(2012KJ20)资助

摘　　要：建立了Fe3+络合-离子对液相色谱-串联质谱法测定纺织品中乙二胺四乙酸(EDTA)和二乙烯三胺五乙酸(DTPA)的残留量。在超声波浴中用NaOH溶液提取纺织品中的EDTA和DTPA,提取液与FeCl3溶液反应生成稳定的络合物,经以四丁基乙酸铵作为阳离子对试剂的C 18柱反相色谱分离后,用电喷雾串联质谱在选择反应监测模式(SRM)下测定。Fe-EDTA和Fe-DTPA的定量离子对分别为m/z 344/300和m/z 445/313,定量限(S/N=10)都为5.0 mg/kg,对6种不同的空白纤维纺织品的添加回收率分别为85.6%～99.3%和85.8%～99.7%,批间RSD分别为1.7%～8.8%和1.1%～8.6%(n=5)。5家外部实验室间2块参考样品中的EDTA和DTPA检测结果的RSD值都小于9%,表明本方法准确、稳定、可靠。An ion-paired liquid chromatography-tandem mass spectrometric method was developed to determine the complexing agents extracted from textiles.EDTA and DTPA firstly were extracted by sodium hydrogen solution under ultrasonic water bath,and then chelated with chlorinated ferric solution,finally separated by the c18-column reversed-phase liquid chromatography with tert-butyl ammonium acetate as AN ion-pairing regent added into mobile phase and determined by electrospray tandem mass spectrometry（ESI-MS/MS） under selective reaction monitoring（SRM） mode.The quantification transitions of Fe-EDTA and Fe-DTPA were m/z 344/300 and m/z 445/313,respectively,AND their limits of quantifications（LOQs）（S/N=10） were both 5.0 mg/kg.In recoverIES experiments for 6 types of fabric,the recovery of EDTA and DTPA WERE IN the ranges of 85.6%～99.3% and 85.8%～99.7%,and their relative standard deviations（RSDs） were at 1.7%～8.8% and 1.1%～8.6%（n=5）,respectively.Five laboratories were invited to take part in the validation of the method,and all inter-lab RSDs were less than 9%.All the results demonstrated the accuracy,stability and reliability of the investigated method.

关 键 词：纺织品 乙二胺四乙酸盐(EDTA) 二乙烯三胺五乙酸盐(DTPA) 液相色谱-串联质谱 络合反应 离子对色谱 

分 类 号：O657.63[理学—分析化学]