【引用本文】 熊茂富, 任敏, 杜伊, 等. 顶空固相微萃取-气相色谱/质谱联用法同时测定湖库水中12种氯苯甲醚的条件优化[J]. 岩矿测试, 2019, 38(6): 724-733. doi: 10.15898/j.cnki.11-2131/td.201901210016
XIONG Mao-fu , REN Min , DU Yi , et al. 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

顶空固相微萃取-气相色谱/质谱联用法同时测定湖库水中12种氯苯甲醚的条件优化

1. 首都师范大学资源环境与旅游学院, 北京 100048;

2. 水利部信息中心, 北京 100053

收稿日期: 2019-01-21  修回日期: 2019-06-10 

基金项目: 国家自然科学基金项目(21377168,41271495);北京市自然科学基金委员会-北京市教育委员会联合资助项目(KZ201810028047)

作者简介: 熊茂富,硕士研究生,环境科学专业。E-mail:15516186738@163.com。。

通信作者:

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

1. College of Resources, Environment and Tourism, Capital Normal University, Beijing 100048, China;

2. Information Center of the Ministry of Water Resources, Beijing 100053, China

Corresponding author: WANG Xiao-yan , 主要从事非点源污染、环境微生物等方面研究。wangxy@cnu.edu.cn。

Received Date: 2019-01-21
Revised Date: 2019-06-10

摘要:氯苯甲醚类化合物(CAs)是地表水中普遍存在的嗅味物质,在世界各地水环境中均可发现CAs的存在,CAs易在食物链中富集和放大,且随着氯原子取代数增加其毒性逐渐增强。水体中CAs属于痕量物质,检测时需要先对其进行富集处理,以往研究大多是对单个物质进行检测。本文建立了采用顶空固相微萃取结合气相色谱-质谱联用技术同时测定湖库水中12种CAs的方法。实验中对顶空固相微萃取过程中的萃取纤维、萃取温度、离子强度、萃取时间及搅拌速率等条件进行对比和优化,确认了最佳萃取条件为:萃取温度80℃,离子浓度0.35g/mL,萃取时间40min,搅拌速率1150r/min,样品体积10mL(15mL萃取瓶)。采用气相色谱-质谱选择性离子扫描方式进行定量分析,方法的线性范围为1~50ng/L,检出限均低于0.18ng/L,回收率为95.5%~115.1%,相对标准偏差小于13.02%。该方法相较于固相萃取及吹扫捕集法的检出限更低,对于样品浓度的变化感应度高,实验仪器的精密度优于其他方法。

关键词: 氯苯甲醚, 顶空固相微萃取, 气相色谱-质谱法, 萃取条件

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

KEY WORDS: chloroanisoles, headspace solid phase microextraction, gas chromatography-mass spectrometry, extraction conditions

本文参考文献

[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.

[2]

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

[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.

[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.

[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.

[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.

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.

[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.

[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):0-349.

[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.

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.

[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.

[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.

[12]

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

[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.

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.

[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.

[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.

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.

[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.

[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.

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.

[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.

[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.

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.

[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.

[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 Chromatography A,2011,1218(12):1576-1584.

[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.

[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.

[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.

[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.

[26]

Chen X,Luo Q,Yuan S,et al.Simultaneous determination 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.

[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.

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.

[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.

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

[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.

[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.

[31]

吴采樱.固相微萃取[M].北京:化学工业出版社,2012:85-107. Wu C Y.Solid Phase Microextraction[M].Beijing:Chemical Industry Press,2012:85

-107.

[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.

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.

[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.

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.

[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.

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.

[35]

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

[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.

[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.

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.

[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.

Chen C,Li Yan,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.

[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. 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.

[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.

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.

[41]

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

[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.

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.

[43]

齐美玲.气相色谱分析及应用[M].北京:科学出版社,2012. Qi M L.Gas Chromatography Analysis and Application[M].Beijing:Science Press,2012.

[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.

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.

[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.

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.

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顶空固相微萃取-气相色谱/质谱联用法同时测定湖库水中12种氯苯甲醚的条件优化

熊茂富, 任敏, 杜伊, 赵高峰, 王晓燕