ASE-GPC-GC/MS同时测定土壤中16种苯胺类物质
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摘要
该文建立了快速溶剂萃取(ASE)-凝胶色谱净化(GPC)-气相色谱/质谱法(GC/MS)测定土壤中16种苯胺类化合物的分析方法。采用正己烷/丙酮(1∶1,V/V)为萃取溶剂提取,凝胶色谱净化,经HP-5MS(30.0 m×0.25 mm×0.25μm)色谱柱分离,质谱检测器检测,外标法定量。实验结果表明,16种苯胺类化合物在0.5～10 mg/L间具有良好的线性,相关系数(R)均>0.999。取样量为10.0 g时,16种苯胺类化合物的方法检出限(MDLs)在0.021～0.076 mg/kg之间。在空白基底中进行加标回收实验,回收率在82.2%～96.1%之间,精密度(RSD)均<10%。实际土壤样品的加标回收率为79.4%～90.1%。该方法前处理简便,准确、稳定,能够满足土壤中多种苯胺类化合物的同时测定。
A method based on gas chromatography/mass spectrometry(GC/MS) was developed for the simultaneous determination of 16 aniline compounds in soil. Accelerated solvent extraction(ASE) and gel permeation chromatography(GPC) were used for pretreatment. Samples were extracted with hexane/acetone(1∶1, V/V), then purified with GPC after concentration and solvent exchange. The analytes were isolated with HP-5 MS column(30.0 m×0.25 mm×0.25 μm) and determined by MS.Results showed that all 16 aniline compounds showed great linearity(R>0.999) in the range of 0.5～10 mg/L. The method detection limits(MDLs) of 16 aniline compounds ranged from 0.021 to 0.076 mg/kg with 10.0 g sampling weight. On the basis of blank sample, values of recovery were ranged from 82.2%～96.1%, with the relative standard deviations(RSDs) less than 10%. The average recoveries of practical samples were in the range of 79.4%～90.1%. The established method with convenient pretreatment process is proved to be accurate and stable which is suitable for determination of simultaneous determination of multiple aniline compounds in soil.
A method based on gas chromatography/mass spectrometry(GC/MS) was developed for the simultaneous determination of 16 aniline compounds in soil. Accelerated solvent extraction(ASE) and gel permeation chromatography(GPC) were used for pretreatment. Samples were extracted with hexane/acetone(1∶1, V/V), then purified with GPC after concentration and solvent exchange. The analytes were isolated with HP-5 MS column(30.0 m×0.25 mm×0.25 μm) and determined by MS.Results showed that all 16 aniline compounds showed great linearity(R>0.999) in the range of 0.5～10 mg/L. The method detection limits(MDLs) of 16 aniline compounds ranged from 0.021 to 0.076 mg/kg with 10.0 g sampling weight. On the basis of blank sample, values of recovery were ranged from 82.2%～96.1%, with the relative standard deviations(RSDs) less than 10%. The average recoveries of practical samples were in the range of 79.4%～90.1%. The established method with convenient pretreatment process is proved to be accurate and stable which is suitable for determination of simultaneous determination of multiple aniline compounds in soil.
引文
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[4]周琛,骆春迎,余辉菊,等.直接进样-液相色谱-串联质谱法同时测定水中的5种苯胺类化合物[J].分析化学, 2016,44(6):935-941.Zhou Chen, Luo Chunying, Yu Huiju, et al. Determination of aniline compounds in water by direct injection-liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Analytical Chemistry, 2016,44(6):935-941.
[5]郝全龙,谯华,周从直,等.腐殖质吸附土壤有机污染物研究进展[J].当代化工, 2014,43(10):2068-2071.Hao Quanlong, Qiao Hua, Zhou Congzhi, et al. Research progress in soil organic pollutants adsorption by humus[J].Contemporary Chemical Industry, 2014,43(10):2068-2071.
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[7]曾跃春,高彦征,凌婉婷,等.土壤中有机污染物的形态及植物可利用性[J].土壤通报, 2009,40(6):1479-1484.Zeng Yuechun, Gao Yanzheng, Ling Wanting, et al. The residual forms and plant availabilities of organic pollutants in soils[J]. Chinese Journal of Soil Science, 2009,40(6):1479-1484.
[8]李海燕,李楠,于丹丹.微波萃取-气质联用测定土壤中的16种多环芳烃[J].环境监控与预警, 2010,2(1):20-23.Li Haiyan, Li Nan, Yu Dandan. Microwave-assisted extraction:GC-MS determination of 16 polycyclic aromatic hydrocarbons in soils[J]. Environmental Monitoring and Forewarning, 2010,2(1):20-23.
[9]李丽君,王娜,王海娇,等.索氏提取-气质联用同时测定土壤中7种多氯联苯[J].分析试验室, 2009,28(S2):4-7.Li Lijun, Wang Na, Wang Haijiao, et al. Soxhlet extractionGC-MS simultaneous determination of 7 PCBs in soils[J].Chinese Journal of Analysis Laboratory, 2009,28(S2):4-7.
[10]李刚,程柯森,丁波涛.超声萃取分离-气相色谱-质谱法测定土壤中的3种酰胺类化合物含量[J].理化检验(化学分册), 2016,52(6):687-690.Li Gang, Cheng Kesen, Ding Botao. GC-MS determination of 3 amide compounds in soil with separation by ultrasonic extraction[J]. Physical Testing and Chemical Analysis-Part B:Chemical Analysis, 2016,52(6):687-690.
[11]张丽,刘腾飞,杨代凤,等.分散固相萃取-气相色谱测定土壤中有机磷农药[J].环境科学与技术, 2015,38(10):134-139.Zhang Li, Liu Tengfei, Yang Daifeng, et al. Determination of organophosphorus pesticides in soil by gas chromatography with dispersive solid phase extraction[J]. Environmental Science&Technology, 2015,38(10):134-139.
[12]宋晓娟,李海燕,尹明明,等.快速溶剂萃取-气相色谱-串联质谱法分析海洋沉积物中的16种多环芳烃[J].色谱,2018,36(2):51-58.Song Xiaojuan, Li Haiyan, Yin Mingming, et al. Determination of 16 polycyclic aromatic hydrocarbons in marine sediments by gas chromatography-tandem mass spectrometry with accelerated solvent extraction[J]. Chinese Journal of Chromatography, 2018,36(2):51-58.
[13]梁焱,陈盛,张鸣珊,等.快速溶剂萃取-气相色谱-质谱法测定土壤中24种半挥发性有机物含量[J].理化检验(化学分册), 2016,52(6):677-683.Liang Yan, Chen Sheng, Zhang Mingshan, et al. GC-MS determination of 24 semi-volatile organic compounds in soil with accelerated solvent extraction[J]. Physical Testing and Chemical Analysis-Part B:Chemical Analysis, 2016,52(6):677-683.
[14]祝子铜,雷美康,彭芳,等.快速溶剂萃取-凝胶渗透色谱净化-LC/MS/MS结合测定蜂花粉中硝基咪唑类药物[J].药物分析杂志, 2016,36(3):522-529.Zhu Zitong, Lei Meikang, Peng Fang, et al. Determination of nitroimidazoles residues in bee pollen using LC-MS/MS coupled with accelerated solvent extraction and gel permeation chromatographic purification[J]. Chinese Journal of Pharmaceutical Analysis, 2016,36(3):522-529.
[15]陈啟荣,郎爽,魏岩,等.加速溶剂萃取-凝胶色谱净化-气质联用测定土壤中15种有机氯农药残留的方法研究[J].分析测试学报, 2010,29(5):473-477.Chen Qirong, Lang Shuang, Wei Yan, et al. Determination of 15 organochlorine pesticides in soil by gas chromatography-mass spectrometry with accelerated solvent extraction and gel permeation chromatography[J]. Journal of Instrumental Analysis, 2010,29(5):473-477.
[2] Dom N, Knapen D, Benoot D, et al. Aquatic multi-species acute toxicity of(chlorinated)anilines:experimental versus predicted data[J]. Chemosphere, 2010,81(2):177-186.
[3]赵云芝,杨坪,钱蜀.液相色谱-串联质谱法测定水中14种苯胺类化合物[J].色谱, 2015,33(5):508-513.Zhao Yunzhi, Yang Ping, Qian Shu. Determination of 14 aniline derivatives in water by liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography,2015,33(5):508-513.
[4]周琛,骆春迎,余辉菊,等.直接进样-液相色谱-串联质谱法同时测定水中的5种苯胺类化合物[J].分析化学, 2016,44(6):935-941.Zhou Chen, Luo Chunying, Yu Huiju, et al. Determination of aniline compounds in water by direct injection-liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Analytical Chemistry, 2016,44(6):935-941.
[5]郝全龙,谯华,周从直,等.腐殖质吸附土壤有机污染物研究进展[J].当代化工, 2014,43(10):2068-2071.Hao Quanlong, Qiao Hua, Zhou Congzhi, et al. Research progress in soil organic pollutants adsorption by humus[J].Contemporary Chemical Industry, 2014,43(10):2068-2071.
[6]崔嵩,付强,李天霄,等.冻融期土壤温度对有机污染物迁移行为的影响[J].水土保持研究, 2016,23(3):314-320.Cui Song, Fu Qiang, Li Tianxiao, et al. Effect of soil temperature on migration behavior of organic pollutants during freeze-thaw period[J]. Research of Soil and Water Conservation, 2016,23(3):314-320.
[7]曾跃春,高彦征,凌婉婷,等.土壤中有机污染物的形态及植物可利用性[J].土壤通报, 2009,40(6):1479-1484.Zeng Yuechun, Gao Yanzheng, Ling Wanting, et al. The residual forms and plant availabilities of organic pollutants in soils[J]. Chinese Journal of Soil Science, 2009,40(6):1479-1484.
[8]李海燕,李楠,于丹丹.微波萃取-气质联用测定土壤中的16种多环芳烃[J].环境监控与预警, 2010,2(1):20-23.Li Haiyan, Li Nan, Yu Dandan. Microwave-assisted extraction:GC-MS determination of 16 polycyclic aromatic hydrocarbons in soils[J]. Environmental Monitoring and Forewarning, 2010,2(1):20-23.
[9]李丽君,王娜,王海娇,等.索氏提取-气质联用同时测定土壤中7种多氯联苯[J].分析试验室, 2009,28(S2):4-7.Li Lijun, Wang Na, Wang Haijiao, et al. Soxhlet extractionGC-MS simultaneous determination of 7 PCBs in soils[J].Chinese Journal of Analysis Laboratory, 2009,28(S2):4-7.
[10]李刚,程柯森,丁波涛.超声萃取分离-气相色谱-质谱法测定土壤中的3种酰胺类化合物含量[J].理化检验(化学分册), 2016,52(6):687-690.Li Gang, Cheng Kesen, Ding Botao. GC-MS determination of 3 amide compounds in soil with separation by ultrasonic extraction[J]. Physical Testing and Chemical Analysis-Part B:Chemical Analysis, 2016,52(6):687-690.
[11]张丽,刘腾飞,杨代凤,等.分散固相萃取-气相色谱测定土壤中有机磷农药[J].环境科学与技术, 2015,38(10):134-139.Zhang Li, Liu Tengfei, Yang Daifeng, et al. Determination of organophosphorus pesticides in soil by gas chromatography with dispersive solid phase extraction[J]. Environmental Science&Technology, 2015,38(10):134-139.
[12]宋晓娟,李海燕,尹明明,等.快速溶剂萃取-气相色谱-串联质谱法分析海洋沉积物中的16种多环芳烃[J].色谱,2018,36(2):51-58.Song Xiaojuan, Li Haiyan, Yin Mingming, et al. Determination of 16 polycyclic aromatic hydrocarbons in marine sediments by gas chromatography-tandem mass spectrometry with accelerated solvent extraction[J]. Chinese Journal of Chromatography, 2018,36(2):51-58.
[13]梁焱,陈盛,张鸣珊,等.快速溶剂萃取-气相色谱-质谱法测定土壤中24种半挥发性有机物含量[J].理化检验(化学分册), 2016,52(6):677-683.Liang Yan, Chen Sheng, Zhang Mingshan, et al. GC-MS determination of 24 semi-volatile organic compounds in soil with accelerated solvent extraction[J]. Physical Testing and Chemical Analysis-Part B:Chemical Analysis, 2016,52(6):677-683.
[14]祝子铜,雷美康,彭芳,等.快速溶剂萃取-凝胶渗透色谱净化-LC/MS/MS结合测定蜂花粉中硝基咪唑类药物[J].药物分析杂志, 2016,36(3):522-529.Zhu Zitong, Lei Meikang, Peng Fang, et al. Determination of nitroimidazoles residues in bee pollen using LC-MS/MS coupled with accelerated solvent extraction and gel permeation chromatographic purification[J]. Chinese Journal of Pharmaceutical Analysis, 2016,36(3):522-529.
[15]陈啟荣,郎爽,魏岩,等.加速溶剂萃取-凝胶色谱净化-气质联用测定土壤中15种有机氯农药残留的方法研究[J].分析测试学报, 2010,29(5):473-477.Chen Qirong, Lang Shuang, Wei Yan, et al. Determination of 15 organochlorine pesticides in soil by gas chromatography-mass spectrometry with accelerated solvent extraction and gel permeation chromatography[J]. Journal of Instrumental Analysis, 2010,29(5):473-477.