吹扫捕集-气相色谱-质谱法联用测定水中典型的嗅味物质
Determination of typical taste and odor compounds in water by purge and trap-gas chromatography-mass spectrometry
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摘要: 本文建立了吹扫捕集-气相色谱-质谱联用法同时测定水中2-甲基异冰片、土臭素、2,4,6-三氯苯甲醚、β-环柠檬醛、2-异丙基-3-甲氧基吡嗪、2-异丁基-3-甲氧基吡嗪、β-紫罗兰酮和二甲基三硫醚等8种典型嗅味物质的方法,为预警嗅味水质突发事件和开展相关研究奠定基础.对8种典型嗅味物质的样品吹扫条件,如:捕集管的型号、吹扫温度、吹扫时间、解析时间及盐效应等进行优化.本实验测定嗅味物质的最佳条件为:样品中加入NaCl的质量浓度为12%(m/V)、样品吹扫温度40℃、吹扫时间20 min、解析时间2 min和解析温度250℃等.通过基质加标实验验证方法的准确度与精密度,8种嗅味物质在1-50 μg·L-1浓度范围内线性良好,相关系数>0.999,方法检出限(LOD)(S/N=3)在0.4-1.7 ng·L-1.在高、低加标浓度水平下,8种典型嗅味物质回收率范围是85.2%-118%,相对标准偏差为1.03%-4.53%.本方法具有较好的准确性、稳定性和实用性,可用于环境水体中嗅味物质的分析.Abstract: A fast, sensitive and solvent-free method for the determination of eight trace taste and odor compounds, including dimethyltrisulfide, β-cyclocitral, 2,4,6-trichloroanisole, geosmin 2-isopropyl-3-methoxypyrazine, 2-isobutyl-3-methoxypyrazine, 2-methylisoborneol and β-ionone in water samples was developed utilizing automatic purge and trap (P&T) coupled with gas chromatography-mass spectrometry (GC-MS). Parameters such as the type of traps, purge time, purge temperature, desorption time and ionic strength were optimized. Taste and odor compounds (T&O) were purged from 40 mL water sample containing sodium chloride (m/V=12%) at 40℃ for 20 min and desorbed 2 min at 250℃. The calibration curve of these eight T&O showed good linearity in the range of 1-50 μg·L-1 with a correlation coefficient above 0.999. The limits of detection (LOD) (S/N=3) were all below 1.7 ng·L-1. The technique was applied to spiked water samples, and acceptable recoveries were achieved. The recoveries of the analytes from water samples were between 85.2% and 118%, and the relative standard deviations (RSD) were between 1.03% and 4.53% (n=7). This method could be employed for monitoring the eight odors in natural waters with good accuracy, stability and practicability.
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Key words:
- taste and odor compounds /
- purge-and-trap /
- gas chromatography /
- mass spectrometry /
- water
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