色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2015年
5期
508-513
,共6页
液相色谱-串联质谱法%苯胺类化合物%水%直接进样
液相色譜-串聯質譜法%苯胺類化閤物%水%直接進樣
액상색보-천련질보법%분알류화합물%수%직접진양
liquid chromatography-tandem mass spectrometry(LC-MS/MS )%aniline deriva-tives(ADs)%water%direct injection
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。
通過優化色譜和質譜條件，建立瞭直接進樣-液相色譜-串聯四極桿質譜法同時快速檢測水中14種苯胺類化閤物的分析方法。水樣經0.45μm 聚醚砜（ PES）濾膜過濾後，採用 Shim-pack FC-ODS 柱（75 mm ×4.6 mm，3μm）進行分離，以甲醇-0.1％（ v／v）甲痠（35：65，v／v）梯度洗脫，流速0.3 mL／min，柱溫35℃，串聯四極桿質譜的多反應鑑測模式進行檢測。在優化的分析條件下，14種苯胺類化閤物可在12 min內分析完畢，而且線性關繫良好（ r＞0.999），方法檢齣限在0.03~4.19μg／L之間。對加標3箇質量濃度（0.5、5.0、20.0μg／L）的地錶水樣品平行測定6次，14種苯胺類化閤物的相對標準偏差在0.4％~9.4％範圍內。該方法抗榦擾能力彊、分析速度快、靈敏度高，已應用于實際樣品的分析，樣品加標迴收率在68.0％~130％之間。
통과우화색보화질보조건，건립료직접진양-액상색보-천련사겁간질보법동시쾌속검측수중14충분알류화합물적분석방법。수양경0.45μm 취미풍（ PES）려막과려후，채용 Shim-pack FC-ODS 주（75 mm ×4.6 mm，3μm）진행분리，이갑순-0.1％（ v／v）갑산（35：65，v／v）제도세탈，류속0.3 mL／min，주온35℃，천련사겁간질보적다반응감측모식진행검측。재우화적분석조건하，14충분알류화합물가재12 min내분석완필，이차선성관계량호（ r＞0.999），방법검출한재0.03~4.19μg／L지간。대가표3개질량농도（0.5、5.0、20.0μg／L）적지표수양품평행측정6차，14충분알류화합물적상대표준편차재0.4％~9.4％범위내。해방법항간우능력강、분석속도쾌、령민도고，이응용우실제양품적분석，양품가표회수솔재68.0％~130％지간。
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%.
