Professional Committee of Rock and Mineral Testing Technology of the Geological Society of China, National Geological Experiment and Testing CenterHost
2019 Vol. 38, No. 6
Article Contents

Mao-fu XIONG, Min REN, Yi DU, Gao-feng ZHAO, Xiao-yan WANG. Simultaneous Determination of 12 Chloroanisoles in Lake Reservoir Waters by Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry[J]. Rock and Mineral Analysis, 2019, 38(6): 724-733. doi: 10.15898/j.cnki.11-2131/td.201901210016
Citation: Mao-fu XIONG, Min REN, Yi DU, Gao-feng ZHAO, Xiao-yan WANG. Simultaneous Determination of 12 Chloroanisoles in Lake Reservoir Waters by Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry[J]. Rock and Mineral Analysis, 2019, 38(6): 724-733. doi: 10.15898/j.cnki.11-2131/td.201901210016

Simultaneous Determination of 12 Chloroanisoles in Lake Reservoir Waters by Headspace Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry

More Information
  • BACKGROUNDChloroanisoles (CAs) are odorous substances and can easily be found in surface waters. The CAs have been found in water environments worldwide. In the food chain, CAs are easily enriched and amplified. The toxicity increases with the number of chlorine atoms substituted. CAs in waters are trace substances which need to be preconcentrated before determination. Previous studies focused on the detection of individual substances. OBJECTIVESTo establish a method which combines headspace solid phase microextraction and gas chromatography-mass spectrometry together, to simultaneously measure 12 CAs in waters. METHODSThe conditions of extraction fiber, temperature, ionic strength, extraction time and stirring rate were compared and optimized in headspace solid phase microextraction. The optimal extraction conditions were confirmed by the results. Extraction temperature was 80℃, ionic strength was 0.35g/mL, extraction time was 40 minutes, stirring rate was 1150r/min, and sample volume was 10mL (15mL extraction bottle). RESULTSQuantitative analysis was performed by gas chromatography-mass spectrometry with selective ion scanning. The linear ranges of the method were 1-50ng/L, and the recoveries were 95.5%-115.1%. The detection limits were 0.045-0.185ng/L and the relative standard deviation was less than 13.02%. CONCLUSIONSCompared with the solid phase extraction and the purge with trap method, this method has a lower detection limit and higher sensitivity of the sample concentration. Also, the precision of the experimental instrument is relatively better than other methods.
  • 加载中
  • [1] Fischer C, Fischer U.Analysis of cork taint in wine and cork material at olfactory subthreshold levels by solid phase microextraction[J].Journal of Agricultural & Food Chemistry, 1997, 45(6):1995-1997.

    Google Scholar

    [2] Polásková P, Herszage J, Ebeler S E.Wine flavor:Che-mistry in a glass[J].Chemical Society Reviews, 2008, 37(11):2478-2489. doi: 10.1039/b714455p

    CrossRef Google Scholar

    [3] Ribéreau-Gayon P, Glories Y, Maujean A, et al.Hand-book of Enology:The Chemistry of Wine Stabilization and Treatments[M].New Jersey:John Wiley & Sons, 2006.

    Google Scholar

    [4] Yu S, Xiao Q, Zhu B, et al.Gas chromatography-mass spectrometry determination of earthy-musty odorous compounds in waters by two phase hollow-fiber liquid-phase microextraction using polyvinylidene fluoride fibers[J].Journal of Chromatography A, 2014, 1329(3):45-51.

    Google Scholar

    [5] Nystrom A, Grimvall A, Krantzrulcker C, et al.Drinking-water off-flavor caused by 2, 4, 6-trichloroanisole[J].Water Science and Technology, 1992, 25(2):241-249. doi: 10.2166/wst.1992.0058

    CrossRef Google Scholar

    [6] 毛敏敏, 张可佳, 张土乔, 等.大体积浓缩-固相微萃取-气相色谱-质谱联用测定水样中6种典型嗅味物质[J].分析化学, 2013, 41(5):760-765.

    Google Scholar

    Mao M M, Zhang K J, Zhang S Q, et al.Determination of six typical taste and odor compounds using large volume voncentration, solid phase micro-extraction and gas chromatography-mass spectrometry[J].Chinese Journal of Analytical Chemistry, 2013, 41(5):760-765.

    Google Scholar

    [7] Pizarro C, Pérez-del-Notario N, Sáenz-Mateo A, et al.A simple and sensitive vortex assisted liquid-liquid microextraction method for the simultaneous determination of haloanisoles and halophenols in wines[J].Talanta, 2014, 128:1-8. doi: 10.1016/j.talanta.2014.04.005

    CrossRef Google Scholar

    [8] Prescott J, Norris L, Kunst M, et al.Estimating a "consumer rejection threshold" for cork taint in white wine[J]. Food Quality and Preference, 2005, 16(4):345-349. doi: 10.1016/j.foodqual.2004.05.010

    CrossRef Google Scholar

    [9] 任敏, 赵高峰, 王晓燕, 等.环境中氯苯甲醚类污染物研究进展[J].环境工程技术学报, 2017, 7(3):357-365. doi: 10.3969/j.issn.1674-991X.2017.03.050

    CrossRef Google Scholar

    Ren M, Zhao G F, Wang X Y, et al.Research progress of chloroanisoles pollutants in the environment[J].Journal of Environmental Engineering Technology, 2017, 7(3):357-365. doi: 10.3969/j.issn.1674-991X.2017.03.050

    CrossRef Google Scholar

    [10] Lu X, Fan C, Shang J, et al.Headspace solid-phase microextraction for the determination of volatile sulfur compounds in odorous hyper-eutrophic freshwater lakes using gas chromatography with flame photometric detection[J].Microchemical Journal, 2012, 104:26-32. doi: 10.1016/j.microc.2012.04.001

    CrossRef Google Scholar

    [11] Cheng Y, Ekker M, Chan H M.Relative developmental toxicities of pentachloroanisole and pentachlorophenol in a zebrafish model (Danio Rerio)[J].Ecotoxicology & Environmental Safety, 2015, 112:7-14.

    Google Scholar

    [12] International Standard Organization.Cork Stoppers-Determination of Releasable 2, 4, 6-Trichloroanisole (TCA): ISO 20752-2007[S].Switzerland: ISO Copyright Office, 2007.

    Google Scholar

    [13] 孙静, 王锐, 尹大强.顶空固相微萃取-气质联用法同时测定城市水源水中的九种嗅味物质[J].环境化学, 2016, 35(2):280-286.

    Google Scholar

    Sun J, Wang R, Yin D Q.Simultaneous determination of nine taste and odor compounds in source water of Chinese cities by headspace solid phase micro-extraction combined with gas chromatography-mass spectrometry[J].Environmental Chemistry, 2016, 35(2):280-286.

    Google Scholar

    [14] Bellar T A, Lichtenberg J J, Kroner R C.The occurrence of organohalides in chlorinated drinking waters[J].Journal American Water Works Association, 1974, 66(12):703-706. doi: 10.1002/j.1551-8833.1974.tb02129.x

    CrossRef Google Scholar

    [15] 王园园, 宋晓明, 温玉娟, 等.固相萃取-衍生化-气相色谱-质谱联用测定不同水体中类固醇雌激素方法研究[J].岩矿测试, 2017, 36(5):519-528.

    Google Scholar

    Wang Y Y, Song X M, Wen Y J, et al.Determination of steroid estrogens in different water samples using SPE-derivatization coupled with GC-MS[J].Rock and Mineral Analysis, 2017, 36(5):519-528.

    Google Scholar

    [16] Arthur C L, Pawliszyn J.Solid phase microextraction with thermal desorption using fused silica optical fibers[J].Analytical Chemistry, 1990, 62(19):2145-2148. doi: 10.1021/ac00218a019

    CrossRef Google Scholar

    [17] 王丹华, 邢钧, 吴采樱.用自制新型端羟基冠醚固相微萃取涂层快速监测水中痕量多环芳烃[J].分析科学学报, 2003, 19(2):109-112. doi: 10.3969/j.issn.1006-6144.2003.02.003

    CrossRef Google Scholar

    Wang D H, Xing J, Wu C Y.Application of the novel benzon-15-crown-5 sol-gel coating for solid-phase microextraction in rapid determination of trace PAHs in water at nonequilibrium situatins[J].Journal of Analytical Science, 2003, 19(2):109-112. doi: 10.3969/j.issn.1006-6144.2003.02.003

    CrossRef Google Scholar

    [18] Kristiana I, Joll C, Heitz A.Analysis of halonitriles in drinking water using solid-phase microextraction and gas chromatography-mass spectrometry[J].Journal of Chromatography A, 2012, 1225(1):45-54.

    Google Scholar

    [19] 余胜兵, 朱炳辉, 许瑛华, 等.顶空固相微萃取谱-气相色谱-质谱联用测定饮用水中6种致嗅化合物[J].分析试验室, 2013, 32(7):58-62.

    Google Scholar

    Yu S B, Zhu B H, Xu Y H, et al.Determination of six earthy musty odorous compounds in drinking water by headspace solid-phase microextraction coupled with gas chromatography-mass spectroscopy[J].Chinese Journal of Analysis Laboratory, 2013, 32(7):58-62.

    Google Scholar

    [20] Vestner J, Fritsch S, Rauhut D.Development of a microwave assisted extraction method for the analysis of 2, 4, 6-trichloroanisole in cork stoppers by SIDA-SBSE-GC-MS[J].Analytica Chimica Acta, 2010, 660(1):76-80.

    Google Scholar

    [21] Pizarro C C, Sáenz-González N, Pérez-del-Notario, et al.Development of a dispersive liquid-liquid microextraction method for the simultaneous determination of the main compounds causing cork taint and brett character in wines using gas chromatography-tandem mass spectrometry[J].Journal of Chromato-graphy A, 2011, 1218(12):1576-1584. doi: 10.1016/j.chroma.2011.01.055

    CrossRef Google Scholar

    [22] Martínez-Uruñuela A, González-Sáiz J M, Pizarro C.Optimisation of a headspace solid-phase microextraction method for the direct determination of chloroanisoles related to cork taint in red wine[J].Journal of Chromatography A, 2004, 1056(1):49-56.

    Google Scholar

    [23] Pizarro C, Pérez-del-Notario N, González-Sáiz J M.Multiple headspace solid-phase microextraction for eliminating matrix effect in the simultaneous determination of haloanisoles and volatile phenols in wines[J].Journal of Chromatography A, 2007, 1166(1):1-8.

    Google Scholar

    [24] Yu S, Qin X, Zhu B, et al.Gas chromatography-mass spectrometry determination of earthy-musty odorous compounds in waters by two phase hollow-fiber liquid-phase microextraction using polyvinylidene fluoride fibers[J].Journal of Chromatography A, 2014, 1329(3):45-51.

    Google Scholar

    [25] Apostolou T, Pascual N, Marco M, et al.Extraction-less, rapid assay for the direct detection of 2, 4, 6-trichloroanisole (TCA) in cork samples[J].Talanta, 2014, 125:336-340. doi: 10.1016/j.talanta.2014.03.023

    CrossRef Google Scholar

    [26] Chen X, Luo Q, Yuan S, et al.Simultaneous determina-tion of ten taste and odor compounds in drinking water by solid-phase microextraction combined with gas chromatography-mass spectrometry[J].Journal of Environmetal Sciences, 2013, 25(11):2313-2323. doi: 10.1016/S1001-0742(12)60290-3

    CrossRef Google Scholar

    [27] 高松, 邓银舟, 李玉芹, 等.闭合超声循环吹扫针捕集动态提取-气相色谱法测定地下水中的4种有机磷农药[J].岩矿测试, 2015, 34(4):480-486.

    Google Scholar

    Gao S, Deng Y Z, Li Y Q, et al.Determination of organophosphorus pesticides in groundwater by gas chromatography coupled with closed ultrasound circulating purge needle trap[J].Rock and Mineral Analysis, 2015, 34(4):480-486.

    Google Scholar

    [28] 徐洁, 鲜啟鸣.气相色谱-质谱法分析某阻燃剂生产厂周边淡水鱼中的多溴联苯醚及其累积特征[J].岩矿测试, 2017, 36(4):405-412.

    Google Scholar

    Xu J, Xian Q M.Determination of polybrominated diphenyl ethers and bioaccumulation in freshwater fish surrounding a flame retardant manufacturing plant by gas chromatography-mass spectrometry[J].Rock and Mineral Analysis, 2017, 36(4):405-412.

    Google Scholar

    [29] Giansante L, di Vincenzo D, Bianchi G.Classification of monovarietal Italian olive oils by unsupervised (PCA) and supervised (LDA) chemometrics[J].Journal of Science of Food and Agriculture, 2003, 83(9):905-911. doi: 10.1002/jsfa.1426

    CrossRef Google Scholar

    [30] Camino-Sánchez F J, Ruiz-García J, Zafra-Gómez A.Development of a thermal desorption gas chromatography-mass spectrometry method for quantitative determination of haloanisoles and halophenols in wineries' ambient air[J].Journal of Chromatography A, 2013, 13(5):259-266.

    Google Scholar

    [31] 吴采樱.固相微萃取[M].北京:化学工业出版社, 2012:85-107.

    Google Scholar

    Wu C Y.Solid Phase Microextraction[M].Beijing:Chemical Industry Press, 2012:85-107.

    Google Scholar

    [32] 魏魏, 郭庆园, 赵云云, 等.顶空固相微萃取-气质联用法测定水中7种致嗅物质[J].中国给水排水, 2014, 30(18):131-135.

    Google Scholar

    Wei W, Guo Q Y, Zhao Y Y, et al.Simultaneous determination of seven fishy aldehydes in water samples using headspace solid-phase microextraction coupled with gas chromatography/mass spectrometry[J].China Water and Wastewater, 2014, 30(18):131-135.

    Google Scholar

    [33] 张哲琦, 牟德华, 李艳.优化GC检测2, 4, 6-三氯苯甲醚的萃取条件[J].食品工业科技, 2014, 35(24):89-95.

    Google Scholar

    Zhang Z Q, Mou D H, Li Y.Optimization of extraction conditions of 2, 4, 6-trichloroanisole determination by gas chromatography[J].Science and Technology of Food Industry, 2014, 35(24):89-95.

    Google Scholar

    [34] 徐振秋, 张晓赟, 徐恒省.顶空固相微萃取-气相色谱-质谱法测定饮用水中9种嗅味物质[J].化学分析计量, 2017, 26(2):48-51. doi: 10.3969/j.issn.1008-6145.2017.02.013

    CrossRef Google Scholar

    Xu Z Q, Zhang X Z, Xu H S.Detection of nine odor compounds in drinking water by headspace solid phase micro-extraction coupled with gas chromatography-mass spectrometry[J].Chemistry Analysis and Meterage, 2017, 26(2):48-51. doi: 10.3969/j.issn.1008-6145.2017.02.013

    CrossRef Google Scholar

    [35] Buchholz K D, Pawliszyn J.Optimization of solid-phase microextraction conditions for determination of phenols[J].Analytical Chemistry, 1994, 66(1):160-167. doi: 10.1021/ac00073a027

    CrossRef Google Scholar

    [36] Zalacain A, Alonso G L, Lorenzo C, et al.Stir bar sorptive extraction for the analysis of wine cork taint[J].Journal of Chromatography A, 2004, 1033(1):173-178. doi: 10.1016/j.chroma.2003.12.059

    CrossRef Google Scholar

    [37] 宋荣娜, 杨晓芳, 吕明晗, 等.HS-SPME-GC/MS同时测定污废水中多种VOCs异味物质[J].环境化学, 2019, 38(5):1047-1056.

    Google Scholar

    Song R N, Yang X F, Lü M H, et al.Simultaneous determination of various odorous VOC substances in sewage wastewater by HSSPME-GC/MS[J].Environmental Chemistry, 2019, 38(5):1047-1056.

    Google Scholar

    [38] 陈臣, 李艳, 牟德华.优化GC检测欧李酒香气成分的萃取条件[J].食品工业科技, 2014, 35(6):81-86.

    Google Scholar

    Chen C, Li Y, Mou D H.Optimization extraction conditions for GC analysis of aromatic constituents in prunus humilis bunge wine[J].Science and Technology of Food Industry, 2014, 35(6):81-86.

    Google Scholar

    [39] 范苓, 秦宏兵, 张晓赟.顶空固相微萃取-气相色谱/质谱法同时测定富营养化水体中9种异味物质[J].江南大学学报(自然科学版), 2014, 13(3):355-359. doi: 10.3969/j.issn.1671-7147.2014.03.019

    CrossRef Google Scholar

    Fan L, Qin H B, Zhang X Z.Determination of nine off-flavor compounds in water by gas chromatography-mas spectrometry with headspace solid phase micro-extraction[J].Journal of Jiangnan University (Natural Science Edition), 2014, 13(3):355-359. doi: 10.3969/j.issn.1671-7147.2014.03.019

    CrossRef Google Scholar

    [40] 马康, 张金娜, 何雅娟, 等.顶空固相微萃取-气质联用测定环境水样中7种痕量土霉味物质[J].分析化学, 2011, 39(12):1823-1829.

    Google Scholar

    Ma K, Zhang J N, He Y J, et al.Determination of seven musty odor compounds in water by gas chromatography mass spectrometry with headspace solid phase micro-extraction[J].Chinese Journal of Analytical Chemistry, 2011, 39(12):1823-1829.

    Google Scholar

    [41] Whitfield F B, Hill J L, Shaw K J.2, 4, 6-tribromoani-sole:A potential cause of mustiness in packaged food[J].Journal of Agricultural and Food Chemistry, 1997, 45(3):889-893. doi: 10.1021/jf960587u

    CrossRef Google Scholar

    [42] 赵英莲, 牟德华, 李艳, 等.顶空固相微萃取联合气相色谱-质谱检测葡萄酒中2, 4, 6-三氯苯甲醚[J].食品科学, 2016, 37(10):219-225. doi: 10.7506/spkx1002-6630-201610038

    CrossRef Google Scholar

    Zhao Y L, Mou D H, Li Y, et al.Optimization of headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry for the determination of 2, 4, 6-trichloroanisole in wine[J].Food Science, 2016, 37(10):219-225. doi: 10.7506/spkx1002-6630-201610038

    CrossRef Google Scholar

    [43] 齐美玲.气相色谱分析及应用[M].北京:科学出版社, 2012.

    Google Scholar

    Qi M L.Gas Chromatography Analysis and Application[M].Beijing:Science Press, 2012.

    Google Scholar

    [44] 沈斐, 苏晓燕, 许燕娟, 等.吹扫捕集-GC/MS法测定饮用水中致嗅物质[J].环境监测管理与技术, 2010, 22(5):31-35. doi: 10.3969/j.issn.1006-2009.2010.05.008

    CrossRef Google Scholar

    Shen F, Su X Y, Xu Y J, et al.Determination of odor materials in drinking water by GC/MS with purge and trap[J].The Administration and Technique of Environmental Monitoring, 2010, 22(5):31-35. doi: 10.3969/j.issn.1006-2009.2010.05.008

    CrossRef Google Scholar

    [45] 唐熙, 梁鸣, 李小晶, 等.气相色谱-质谱法测定软木塞中2种霉味物质[J].色谱, 2012, 30(7):733-737.

    Google Scholar

    Tang X, Liang M, Li X J, et al.Determination of two mouldy compounds in cork by gas chromatography-mass spectrometry[J].Chinese Journal of Chromatography, 2012, 30(7):733-737.

    Google Scholar

  • 加载中
通讯作者: 陈斌, bchen63@163.com
  • 1. 

    沈阳化工大学材料科学与工程学院 沈阳 110142

  1. 本站搜索
  2. 百度学术搜索
  3. 万方数据库搜索
  4. CNKI搜索

Figures(3)

Tables(2)

Article Metrics

Article views(3610) PDF downloads(104) Cited by(0)

Access History

Other Articles By Authors

Catalog

    /

    DownLoad:  Full-Size Img  PowerPoint