色谱2016，Vol.34Issue(3)：289-298,10.DOI:10.3724/SP.J.1123.2015.11009
固相萃取／液相色谱-串联质谱法测定水中苯胺类化合物及基质干扰的消除
Determination of aniline derivatives in water by solid phase extraction/liquid chromatography-tandem mass spectrometry and elimination of matrix interference
摘要
Abstract
A method was developed for the determination of 18 aniline derivatives( ADs ) in water by liquid chromatography-tandem mass spectrometry( LC-MS/MS)coupled with solid phase extraction. The water sample was enriched by a mixed cation exchange column( MCX) and a silicon substrate cation exchange column( SCX ). The column was eluted by ammonia methanol solution. The eluent was concentrated and then diluted with purified water to the appropriate multiple. The separation of ADs was performed on an ODS column,and the mobile phase of methanol-0. 005%( v/v)formic acid aqueous solution was employed with gradient elu-tion,then the analytes were detected by LC-MS/MS in multiple reaction monitoring mode,with internal standard method for quantitative analysis. The analysis of the 18 ADs was completed in 15 min and the calibration curves showed good linearity. When an MCX was employed for extraction,the method detection limits of the 16 ADs ranged from 0. 002 to 0. 035 μg/L,the average recoveries and relative standard deviations of the 16 ADs in surface water were 72. 5%-92. 5%( n=6)and 1. 4%-9. 6%( n=6),respectively. When an SCX was employed for extrac-tion,the method detection limits of the 17 ADs ranged from 0. 013 to 0. 207 μg/L,and the aver-age recoveries and relative standard deviations of the 17 ADs in surface water were 66. 5%-102%( n=6)and 2. 4%-13. 6%( n=6),respectively. During the development of this method, five elimination methods of matrix interference were studied. The results showed that adjust-ment of chromatographic separation conditions is the most efficient method,and the selection of appropriate method for sample preparation is the second one. The replacement of ion source ,internal standard method and calibration by matrix matched standard solution can elim-inate and compensate matrix interference to some extent.关键词
固相萃取/液相色谱-串联质谱法/消除基质干扰的方法/苯胺类化合物/水样Key words
solid phase extraction( SPE)/liquid chromatography-tandem mass spectrometry(LC-MS/MS)/elimination methods of matrix interference/aniline derivatives( ADs)/water分类
化学化工引用本文复制引用
赵云芝,谢振伟,潘乐丹,姚欢..固相萃取／液相色谱-串联质谱法测定水中苯胺类化合物及基质干扰的消除[J].色谱,2016,34(3):289-298,10.基金项目
国家环境保护标准项目（2014-34）．@@@@Establishment of National Standards for Environmental Protection（ No．2014-34）． （）
