顶空-气相色谱-质谱法测定水中氯代苯胺类化合物
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摘要
提出用顶空采样法富集水样中12种氯代苯胺类化合物,经气相色谱分离后用质谱法测定其含量。试验选择了最佳顶空条件。取水样8.00mL置于顶空瓶中,加入碳酸钠3.4g(盐析剂)和0.500mg·L-1内标溶液8μL,于80℃恒温条件下振荡40min。测定的12种化合物以气体状态进入DB-35MS色谱柱,按程序升温模式进行分离;质谱测定中,采用电子轰击离子源和选择离子监测模式。12种氯代苯胺类化合物的质量浓度在一定范围内与其峰面积呈线性关系,其检出限(3.14s)在0.03～0.3μg·L-1之间。按标准加入法进行回收试验,测得回收率在86.0%～131%之间,测定值的相对标准偏差(n=6)在3.0%～20%之间。
Headspace(HS)sampling was applied to enrich 12 chloroanilines in water samples,and the analytes were then separated by GC and determined by MS.Optimum conditions for HS treatment were studied in detail.8.00 mL of the water sample were placed in the HS-flask,and 3.4 g of Na2 CO3(as salting-out reagent)together with 8μL of 0.500 mg·L-1 internal standard solution were added.The mixture was shaken for 40 min at constant temperature of 80℃.12 chloroanilines to be determined were introduced into DB-35 MS chromatographic column from the HS-flask and separated under the mode of programmed temperature elevation.In MS analysis,EI and SIM mode were adopted.Linear relationships between values of peak area and mass concentration of the 12 chloroanilines were found in definite ranges,and the detection limits(3.14 s)were found in the range of 0.03-0.3μg·L-1.Recovery was tested by standard addition method,giving results of recovery in the range of 86.0%-131%.Values of RSDs(n=6)ranged from 3.0%to 20%.
Headspace(HS)sampling was applied to enrich 12 chloroanilines in water samples,and the analytes were then separated by GC and determined by MS.Optimum conditions for HS treatment were studied in detail.8.00 mL of the water sample were placed in the HS-flask,and 3.4 g of Na2 CO3(as salting-out reagent)together with 8μL of 0.500 mg·L-1 internal standard solution were added.The mixture was shaken for 40 min at constant temperature of 80℃.12 chloroanilines to be determined were introduced into DB-35 MS chromatographic column from the HS-flask and separated under the mode of programmed temperature elevation.In MS analysis,EI and SIM mode were adopted.Linear relationships between values of peak area and mass concentration of the 12 chloroanilines were found in definite ranges,and the detection limits(3.14 s)were found in the range of 0.03-0.3μg·L-1.Recovery was tested by standard addition method,giving results of recovery in the range of 86.0%-131%.Values of RSDs(n=6)ranged from 3.0%to 20%.
引文
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[3] SUSARLA S, MASUNAGA S, YONEZAWA Y.Transformations of chloronitrobenzenes in anaerobic sediment[J].Chemosphere,1996,32(5):967-977.
[4] XIAO Y,LIU R,ZHAO X,et al.Characterization of genes involved in the initial reactions of 4-chloronitrobenzene degradation in pseudomonas putida ZWL73[J].Applied Microbiology and Biotechnology,2006,73(1):166-171.
[5]国家环境保护总局《水和废水监测分析方法》编委会.水和废水监测分析方法[M].4版.北京:中国环境科学出版社,2006.
[6]张雁,陈振贺,柯建明,等.在线固相萃取-液质联用法测定地下水中痕量苯胺和联苯胺[J].分析试验室,2015,34(5):541-544.
[7] YANG Q,SU W,JIANG X Y,et al.Application of vortex-assisted supramolecular solvent liquid-liquid microextraction for trace determination of nitroaniline isomers[J].International Journal of Environmental Analytical Chemistry,2014,94(8):812-821.
[8]张建莹,靳保辉,吴卫东,等.超高效液相色谱-串联质谱法测定菠菜、苹果及大豆中二硝基苯胺类除草剂残留量[J].质谱学报,2017,39(1):1-7.
[9]郑美洁,向垒,李彦文,等.液液萃取-气相色谱/质谱法同时测定水中3种季胺盐化合物[J].分析化学研究报告,2014(5):735-740.
[10]张海霞,朱彭龄.固相萃取[J].分析化学,2000(9):1172-1180.
[11]陈烨,王超,许秀艳,等.顶空固相微萃取/气相色谱法快速测定水中氯代苯胺类残留[J].分析测试学报,2014,33(9):1056-1061.
[12] XIE W Q,CHAI X S.Determination of epoxy groups in epoxy resins by reaction-based headspace gas chromatography[J].Polymer Testing,2017,59:113-117.
[13] SNOW N H,SLACK G C.Head-space analysis in modern gas chromatography[J].TrAC-Trends in Analytical Chemistry,2002,21(9/10):608-617.
[14]王永华.顶空气相色谱分析原理与技术[J].中国环境监测,2006,22(2):7-13.
[15] EPA 8131 Aniline and selected derivatives by gas chromatography[S].
[16] PUZIKOV E A,BLAZHEVAL I V,ZILBERMAN B Y,et al.Extraction of nitric acid and uranyl nitrate with tributyl phosphate in diluent in the presence of salting-out agents and its mathematical description[J].Radiochemistry,2013,55(4):369-376.
[17] ZHANG C Y,HU H C,CHAI X S,et al.Determination of maximal amount of minor gases adsorbed in a shale sample by headspace gas chromatography[J].Journal of Chromatography A,2014,1328(7):80-84.
[18]王永华.分配常数及气液相比对顶空气相色谱分析灵敏度的影响[J].北京大学学报,2003,39(6):896-900.
[19] KOLB B,ETTRE L S.Static headspace-gas chromatography-theory and practice[M].New York:WileyVCH Press,2006.
[20] HJ 168-2010分析方法标准制修订技术导则[S].
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