Determination of Odorants of Geosmin, 2-Methylisoborneol and β-Ionone in Source Water of Taihu Lake by Gas Chromatography-Mass Spectrometry after Headspace-Solid Phase Microextraction
摘 要
水样过0.45 μm滤膜,分取10 mL滤液和已经于450℃处理2 h的氯化钠2.5 g混合,在顶空仪中于65℃平衡5 min,再用二乙烯苯基/Carboxen/聚二甲基硅氧烷(DVB/CAR/PDMS)固相微萃取纤维头在500 r·min-1转速下于65℃萃取30 min,于250℃热解吸3 min,所得气体进入气相色谱-质谱仪,在HP-5MS毛细管色谱柱上用升温程序分离,用附电子轰击离子(EI)源的质谱仪检测。结果显示,土臭素、2-甲基异莰醇的质量浓度在2.0~200.0 ng·L-1内,β-紫罗兰酮的质量浓度在1.0~100.0 ng·L-1内分别与其对应的峰面积呈线性关系,检出限(3.36s)分别为1.38,1.12,0.78 ng·L-1;对纯水及太湖水源水进行3个浓度水平的加标回收试验,水源水中3种嗅味物质的检出量分别为1.78,3.07,3.81 ng·L-1,回收率为92.3%~111%,测定值的相对标准偏差(n=6)为0.98%~13%,适用于水源水中嗅味物质的测定。
Abstract
The water sample was passed through a 0.45 μm filter membrane, and an aliquot (10 mL) of the filtrate was mixed with 2.5 g of sodium chloride that had been treated at 450℃ for 2 h. Targets in the sample were extracted by Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS) solid microextraction fiber head at 65℃ for 30 min with rotating speed of 500 r·min-1, and thermally desorbed at 250℃ for 3 min. The obtained gas was introduced into the gas chromatography-mass spectrometer. Separation was performed on HP-5MS chromatographic capillary column with temperature program, and detection for geosmin, 2-methylisoborneol and β-ionone was performed with mass spectrometer equipped with an electron impact ion (EI) source. It was shown that linear relationships between values of the mass concentration and the corresponding peak area were kept in the range of 2.0-200 ng·L-1 (for geosmin and 2-methylisoborneol) and 1.0-100 ng·L-1 (for β-ionone), with detection limits (3.36s) of 1.38, 1.12, 0.78 ng·L-1, respectively. Test for the spiked recovery was carried out on pure water and source water of Taihu lake at the 3 concentration levels, the detected amounts of the 3 odorants in the source water were 1.78, 3.07, 3.81 ng·L-1, and the recovery was found in the range of 92.3%-111%, with RSDs (n=6) of the determined values in the range of 0.98%-13%, indicating that the proposed method was suitable for the determination of odorants in source water.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202205008
所属栏目 工作简报
基金项目 国家自然科学基金项目(51109153)
收稿日期 2021/3/19
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备注何云峰,硕士研究生,主要研究方向为污水处理与回用技术
引用该论文: HE Yunfeng,LI Cuimei,XUE Tianyi. Determination of Odorants of Geosmin, 2-Methylisoborneol and β-Ionone in Source Water of Taihu Lake by Gas Chromatography-Mass Spectrometry after Headspace-Solid Phase Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(5): 542~547
何云峰,李翠梅,薛天一. 顶空固相微萃取-气相色谱-质谱法测定太湖水源水中嗅味物质土臭素、2-甲基异莰醇以及β-紫罗兰酮的含量[J]. 理化检验-化学分册, 2022, 58(5): 542~547
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【4】辛晓东,王明泉,赵清华,等.饮用水嗅味物质检测与控制技术研究进展[J].中国给水排水, 2013,29(14):13-15.
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【7】MA K, ZHANG J N, ZHAO M, et al. Accurate ana-lysis of trace earthy-musty odorants in water by headspace solid phase microextraction gas chromatography-mass spectrometry[J]. Journal of Separation Science, 2012,35(12):1494-1501.
【8】沈丽娟.水体异味来源及致嗅物质检测技术概述[J].环境研究与监测, 2019(1):23-27.
【9】冯桂学,刘莉,顿咪娜,等.固相萃取-气相色谱-质谱法测定水中10种嗅味物质的含量[J].理化检验-化学分册, 2017,53(5):502-506.
【10】康娜,王正萍,王红.顶空-固相微萃取-气质联用测定终端水异味物质[J].工业水处理, 2019,39(4):89-92.
【11】夏雪,陈倩茹,王川,等.顶空固相微萃取-气相色谱-质谱联用测定黑臭水体中的4种主要异味物质[J].环境化学, 2019,38(12):2789-2796.
【12】闫慧敏,韩正双,白雪娟,等.顶空固相微萃取-气相色谱质谱法测定8种嗅味物质[J].供水技术, 2018,12(6):58-61.
【13】陈克云,于建伟,孙道林,等.顶空固相微萃取-气相色谱/质谱法测定水中藻源嗅味物质[J].中国给水排水, 2011,27(12):94-98.
【14】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.
【15】徐振秋,徐恒省.太湖饮用水源地主要嗅味物质污染现状及其防治对策研究[J].污染防治技术, 2017(2):80-82.
【16】徐琛宇,李翠梅,袁祥,等.太湖上山水源地嗅味物质的研究与分析[J].生态与农村环境学报, 2015,31(5):736-742.
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