Citation: ZHAO Yunzhi, XIE Zhenwei, PAN Ledan, YAO Huan. Determination of aniline derivatives in water by solid phase extraction/liquid chromatography-tandem mass spectrometry and elimination of matrix interference[J]. Chinese Journal of Chromatography, ;2016, 34(3): 289-298. doi: 10.3724/SP.J.1123.2015.11009 shu

Determination of aniline derivatives in water by solid phase extraction/liquid chromatography-tandem mass spectrometry and elimination of matrix interference

1.
Sichuan Environmental Monitoring Center, Chengdu 610091, China

Corresponding author: ZHAO Yunzhi,
Received Date: 5 November 2015

Fund Project: 国家环境保护标准项目(2014-34). (2014-34)

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 elution, 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 μ g/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 extraction, the method detection limits of the 17 ADs ranged from 0.013 to 0.207 μ g/L, and the average 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 adjustment 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 eliminate and compensate matrix interference to some extent.
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沈阳化工大学材料科学与工程学院沈阳 110142