色谱 ›› 2015, Vol. 33 ›› Issue (5): 508-513.DOI: 10.3724/SP.J.1123.2015.01005

• 研究论文 • 上一篇    下一篇

液相色谱-串联质谱法测定水中14种苯胺类化合物

赵云芝, 杨坪, 钱蜀   

  1. 四川省环境监测总站, 四川 成都 610091
  • 收稿日期:2015-01-09 发布日期:2015-04-23
  • 通讯作者: 赵云芝
  • 基金资助:

    国家环境保护标准制定项目(2014-34).

Determination of 14 aniline derivatives in water by liquid chromatography-tandem mass spectrometry

ZHAO Yunzhi, YANG Ping, QIAN Shu   

  1. Sichuan Environmental Monitoring Center, Chengdu 610091, China
  • Received:2015-01-09 Published:2015-04-23

摘要:

通过优化色谱和质谱条件,建立了直接进样-液相色谱-串联四极杆质谱法同时快速检测水中14种苯胺类化合物的分析方法。水样经0.45 μm聚醚砜(PES)滤膜过滤后,采用Shim-pack FC-ODS柱(75 mm×4.6 mm, 3 μm)进行分离,以甲醇-0.1%(v/v)甲酸(35:65, v/v)梯度洗脱,流速0.3 mL/min,柱温35 ℃,串联四极杆质谱的多反应监测模式进行检测。在优化的分析条件下,14种苯胺类化合物可在12 min内分析完毕,而且线性关系良好(r>0.999),方法检出限在0.03~4.19 μg/L之间。对加标3个质量浓度(0.5、5.0、20.0 μg/L)的地表水样品平行测定6次,14种苯胺类化合物的相对标准偏差在0.4%~9.4%范围内。该方法抗干扰能力强、分析速度快、灵敏度高,已应用于实际样品的分析,样品加标回收率在68.0%~130%之间。

关键词: 苯胺类化合物, 水, 液相色谱-串联质谱法, 直接进样

Abstract:

A new and fast method was developed for the simultaneous determination of 14 aniline derivatives (ADs) in water by direct injection-liquid chromatography-tandem mass spectrometry (LC-MS/MS) through optimizing chromatographic and mass spectrometric conditions. The water sample was filtered through a 0.45 μm polyether sulfone (PES) microfiltration membrane. The separation was performed on a Shim-pack FC-ODS column (75 mm×4.6 mm, 3 μm) with methanol-0.1%(v/v) formic acid aqueous solution (35:65, v/v) as mobile phases in gradient elution mode. The flow rate was 0.3 mL/min, and the column temperature was 35 ℃. The analytes were detected by LC-MS/MS in multiple reaction monitoring mode. Under the optimized conditions, the analysis of the 14 aniline derivatives was completed within 12 min and the calibration curves showed good linearity with correlation coefficients not less than 0.999. The detection limits of the 14 aniline derivatives ranged from 0.03 μg/L to 4.19 μg/L. The relative standard deviations of the 14 aniline derivatives in the spiked surface water at three levels (0.5, 5.0, 20.0 μg/L) were 0.4%-9.4% (n=6). The proposed method has the advantages of good anti-interference ability, rapidness and high sensitivity. It was successfully applied to the analysis of real samples, and the recoveries of the 14 aniline derivatives in the spiked real samples were 68.0%-130%.

Key words: aniline derivatives (ADs), direct injection, liquid chromatography-tandem mass spectrometry (LC-MS/MS), water

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