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
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
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摘要: 建立了顶空固相微萃取-气相色谱-质谱联用(HSPME-GC-MS)的分析方法同时检测城市水源水中的9种痕量嗅味物质,具体包括6种土霉味物质(2-甲基异莰醇、土嗅素、2-异丙基-3-甲氧基吡嗪、2-异丁基-甲氧基吡嗪、2-甲基苯并呋喃和2,4,6-三氯苯甲醚)及3种其他种类的嗅味物质(1种鱼腥味物质反,反-2,4-庚二烯醛,1种干草味物质β-环柠檬醛和1种芳香味物质β-紫罗兰酮).在水浴加热搅拌的条件下,利用固相微萃取纤维顶空吸附水中挥发出的嗅味物质,随后在GC-MS上进行物质解吸并检测.本研究对比了不同HSPME萃取纤维的萃取效果,并优化了萃取时间、萃取温度及解吸温度等前处理及仪器条件.研究得到的最优检测条件为:2 cm 50/30μm DVB/CAR/PDMS萃取纤维,在65℃下加热30 min,并于GC进样口解吸3 min.9种嗅味物质在1-200 ng·L-1范围内线性良好,方法检出限为1.36-7.70 ng·L-1,其中8种嗅味物质的检出限均低于3.3 ng·L-1,对水源水的加标回收率为57.7%-94.8%.测定3个不同城市水源水样品中的嗅味物质浓度, 9种物质在水源水中均有检出.除太湖中所含的MIB外,其余水体中MIB及所有水体中的GSM均超过了《生活饮用水卫生标准》(GB5749-2006)中所规定的值.实验证明,HSPME-GC-MS可满足城市水源水中9种痕量嗅味物质的同时检测.Abstract: Headspace solid phase micro-extraction with gas chromatography combined with mass spectrometry(HSPME-GC-MS) was used to analyze nine taste and odor compounds(T&O), including six compounds with earthy and musty odors(i.e., 2-Methylisoborneol, trans-1,10-dimethyl-trans-9-decalol, 2-Isopropyl-3-Methoxypyrazine, 2-Isobutyl-3-Methoxypyrazine, 2-Methylbenzofuran, and 2,4,6-Trichloroanisole), and three compounds with other taste and odors(i.e., trans,trans-2,4-heptandienal with fishy odor, β-Cyclocitral with hay odor, and β-Ionone with flowery odor) in drinking water sources analyze. HSPME fiber was used to adsorb T & O evaporated from the water sample under water bath condition with stirring. After extraction, HSPME fiber was injected into GC-MS for desorption and analysis. We tested the relative extraction efficiencies using different HSPME fibers and under varied operation conditions(i.e., extraction time, extraction temperature, and desorption time). The optimal procedure was obtained as follows:2 cm 50/30μm DVB/CAR/PDMS fiber, 30 min extraction under 65℃, and desorption for 3 min in GC injection port. All the nine T & O exhibited good linear relationships within the range of 1-200 ng·L-1,and the detection limits were between 1.36 and 7.70 ng·L-1(eight T & O were below 3.3 ng·L-1). The recoveries of those source water samples were between 57.7% and 94.8%. The tested nine T & O were all detected in the source water of three cities. The MIB and GSM levels in all source water samples exceeded the limits of national standards for drinking water quality(GB5749-2006), except the MIB concentration in Taihu Lake. Our study supported that HSPME-GC-MS is an ideal method for simultaneous determination of nine T & O in source water of Chinese cities.
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