材料期刊网

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0.45μm 聚醚砜（ PES）滤膜过滤后，采用 Shim-pack FC-ODS 柱（75 mm ×4.6 mm，3μm）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0.03~4.19μg／L之间。对加标3个质量浓度（0.5、5.0、20.0μg／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。

A new and fast method was developed for the simultaneous determination of 14 ani-line derivatives( ADs)in water by direct injection-liquid chromatography-tandem mass spec-trometry( LC-MS/MS)through optimizing chromatographic and mass spectrometric conditions. The water sample was filtered through a 0. 45 μm polyether sulfone( PES)microfiltration mem-brane. The separation was performed on a Shim-pack FC-ODS column( 75 mm × 4. 6 mm,3μm)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 opti-mized 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 analy-sis of real samples,and the recoveries of the 14 aniline derivatives in the spiked real samples were 68. 0%-130%.