气相色谱法测定鄱阳湖湿地多种环境介质中五氯酚钠
|
摘要
采用气相色谱法测定鄱阳湖湿地的沉积物、灰化苔草和水等环境介质中五氯酚钠的含量。样品酸化后采用正己烷萃取,碳酸钾溶液反萃取,乙酸酐衍生化,正己烷提取五氯酚钠衍生物,采用气相色谱-质谱法进行定性分析,采用气相色谱法进行定量分析。气相色谱法测定中用WondaCAP 1色谱柱(30m×0.32mm,0.25μm)分离,电子捕获检测器检测。五氯酚钠的质量浓度在50.0～2 000ng·L~(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)为15.0ng·L~(-1)。加标回收率为94.1%～106%,测定值的相对标准偏差(n=5)为0.50%～2.2%。
GC was applied to the determination of sodium pentachlorophenol in environment media,i.e.sediment,carex cinerascens and water of Poyang lake wetland.After acidification,the sample was extracted with nhexane and then reextracted with potassium carbonate solution.The derivatization was adopted with acetic anhydride and then the derivative was extracted with n-hexane.The quantitative and qualitative analysis were used by GC and GC-MS respectively.The analyte was separated on WondaCAP 1 chromatographic column(30 m×0.32 mm,0.25μm)and detected by ECD in GC determination.Linear relationship between values of peak area and mass concentration of sodium pentachlorophenol was kept in the range of 50.0-2 000 ng·L~(-1),with detection limit(3 S/N)of 15.0 ng·L~(-1).Values of recovery found by standard addition method were in the range of 94.1%-106%,and values of RSDs(n=5)were in the range of 0.50%-2.2%.
GC was applied to the determination of sodium pentachlorophenol in environment media,i.e.sediment,carex cinerascens and water of Poyang lake wetland.After acidification,the sample was extracted with nhexane and then reextracted with potassium carbonate solution.The derivatization was adopted with acetic anhydride and then the derivative was extracted with n-hexane.The quantitative and qualitative analysis were used by GC and GC-MS respectively.The analyte was separated on WondaCAP 1 chromatographic column(30 m×0.32 mm,0.25μm)and detected by ECD in GC determination.Linear relationship between values of peak area and mass concentration of sodium pentachlorophenol was kept in the range of 50.0-2 000 ng·L~(-1),with detection limit(3 S/N)of 15.0 ng·L~(-1).Values of recovery found by standard addition method were in the range of 94.1%-106%,and values of RSDs(n=5)were in the range of 0.50%-2.2%.
引文
[1] MUIR J,EDULJEE G.PCP in the freshwater and marine environment of the European Union[J].The Science of the Total Environment,1999,236:41-56.
[2]谭大,张剑波.Top-down法计算中国五氯酚钠消费分布[J].环境污染与防治,2008(3):17-20.
[3] YU X S,LIU Y,LOU J,et al.Determination of water and methanol extractable pentachlorophenol in soils using vortex-assisted liquid-liquid extraction and gas chromatography[J].Chinese Journal of Analytical Chemistry,2015,43(9):1389-1394.
[4] AMENDOLA L,CORTESE M,VINATORU D,et al.Innovative analytical method for the determination of underivatize tributyltin and pentachlorophenol in seawater by gas chromatography-triple quadrupole mass spectrometry[J].Analytica Chimica Acta,2017,975:70-77.
[5] DONG J P,LEE T,PARK K Y.Simultaneous determination of bisphenol A,chlorophenols and alkylphenols by solid-phase extraction and HPLC[J].Analytical Science&Technology,2017,30(1):20-25.
[6] KADMI Y,FAVIER L,HARJA M,et al.A new strategy for pentachlorophenol monitoring in water samples using ultra-high performance liquid chromatography-mass spectrometry tandem[J].Environmental Engineering and Management Journal,2015,14(3):567-574.
[7] NESAKUMAR N,GUMPU M B,NAGARAJAN S,et al.Simultaneous voltammetric determination of captan,carbosulfan,2,3,7,8-tetrachlorodibenzodioxin and pentachlorophenol in groundwater by ceria nanospheres decorated platinum electrode and chemometrics[J].Measurement,2017,109:130-136.
[8] WU W Q,XIAO H,LUO S L,et al.A highly stable and effective electrochemiluminescence platform of copper oxide nanowires coupled with graphene for ultrasensitive detection of pentachlorophenol[J].Sensors and Actuators B:Chemical,2016,222:747-754.
[9] HONG H C,ZHOU H Y,LUAN T G,et al.Residue of pentachlorophenol in freshwater sediments and human breast milk collected from the Pearl River Delta,China[J].Environment International,2005,31(5):643-649.
[10] ZHENG M H,ZHANG B,BAO Z C,et al.Analysis of penachlorophenol from water,sediments and fish bile of Dongting Lake in China[J].Bulletin of Environmental Contamination and Toxicology,2000,64:16-19.
[11]曲丽娟,鲜啟鸣,邹惠仙.固相微萃取-气相色谱法测定饮用水及其水源水中的氯酚[J].环境污染与防治,2004(2):154-155.
[12]刘金林,胡建英,万祎,等.海河流域和渤海湾沉积物和水样中五氯酚的分布[J].环境化学,2006,25(5):539-542.
[13] TANG Z W,YANG Z F,SHEN Z Y,et al.Pentachlorophenol residues in suspended particulate matter and sediments from the Yangtze river catchment of Wuhan,China[J].Bulletin of Environmental Contamination and Toxicology,2007,78:158-162.
[14] THUAN N T,TSAI C L,WENG Y M,et al.Analysis of polychlorinated dibenzo-p-dioxins and furans in various aqueous samples in Taiwan[J].Chemosphere,2011,83(6):760-766.
[15]陈春丽,向洪锐,戴星照,等.中国天然水体中五氯酚的浓度水平、管理及来源分析[J].生态毒理学报,2015,10(6):71-79.
[16]刘小真,周文斌,胡利娜,等.鄱阳湖区洲滩底质有机氯农药的垂直污染特征[J].生态环境,2008(4):1348-1353.
[2]谭大,张剑波.Top-down法计算中国五氯酚钠消费分布[J].环境污染与防治,2008(3):17-20.
[3] YU X S,LIU Y,LOU J,et al.Determination of water and methanol extractable pentachlorophenol in soils using vortex-assisted liquid-liquid extraction and gas chromatography[J].Chinese Journal of Analytical Chemistry,2015,43(9):1389-1394.
[4] AMENDOLA L,CORTESE M,VINATORU D,et al.Innovative analytical method for the determination of underivatize tributyltin and pentachlorophenol in seawater by gas chromatography-triple quadrupole mass spectrometry[J].Analytica Chimica Acta,2017,975:70-77.
[5] DONG J P,LEE T,PARK K Y.Simultaneous determination of bisphenol A,chlorophenols and alkylphenols by solid-phase extraction and HPLC[J].Analytical Science&Technology,2017,30(1):20-25.
[6] KADMI Y,FAVIER L,HARJA M,et al.A new strategy for pentachlorophenol monitoring in water samples using ultra-high performance liquid chromatography-mass spectrometry tandem[J].Environmental Engineering and Management Journal,2015,14(3):567-574.
[7] NESAKUMAR N,GUMPU M B,NAGARAJAN S,et al.Simultaneous voltammetric determination of captan,carbosulfan,2,3,7,8-tetrachlorodibenzodioxin and pentachlorophenol in groundwater by ceria nanospheres decorated platinum electrode and chemometrics[J].Measurement,2017,109:130-136.
[8] WU W Q,XIAO H,LUO S L,et al.A highly stable and effective electrochemiluminescence platform of copper oxide nanowires coupled with graphene for ultrasensitive detection of pentachlorophenol[J].Sensors and Actuators B:Chemical,2016,222:747-754.
[9] HONG H C,ZHOU H Y,LUAN T G,et al.Residue of pentachlorophenol in freshwater sediments and human breast milk collected from the Pearl River Delta,China[J].Environment International,2005,31(5):643-649.
[10] ZHENG M H,ZHANG B,BAO Z C,et al.Analysis of penachlorophenol from water,sediments and fish bile of Dongting Lake in China[J].Bulletin of Environmental Contamination and Toxicology,2000,64:16-19.
[11]曲丽娟,鲜啟鸣,邹惠仙.固相微萃取-气相色谱法测定饮用水及其水源水中的氯酚[J].环境污染与防治,2004(2):154-155.
[12]刘金林,胡建英,万祎,等.海河流域和渤海湾沉积物和水样中五氯酚的分布[J].环境化学,2006,25(5):539-542.
[13] TANG Z W,YANG Z F,SHEN Z Y,et al.Pentachlorophenol residues in suspended particulate matter and sediments from the Yangtze river catchment of Wuhan,China[J].Bulletin of Environmental Contamination and Toxicology,2007,78:158-162.
[14] THUAN N T,TSAI C L,WENG Y M,et al.Analysis of polychlorinated dibenzo-p-dioxins and furans in various aqueous samples in Taiwan[J].Chemosphere,2011,83(6):760-766.
[15]陈春丽,向洪锐,戴星照,等.中国天然水体中五氯酚的浓度水平、管理及来源分析[J].生态毒理学报,2015,10(6):71-79.
[16]刘小真,周文斌,胡利娜,等.鄱阳湖区洲滩底质有机氯农药的垂直污染特征[J].生态环境,2008(4):1348-1353.