Division of Chemical Metrology and Analytical Science, National Institute of Metrology of China, Beijing, China.
J Sep Sci. 2012 Jun;35(12):1494-501. doi: 10.1002/jssc.201200029.
A simple and sensitive method was developed for the simultaneous separation and determination of trace earthy-musty compounds including geosmin, 2-methylisoborneol, 2-isobutyl-3-methoxypyrazine, 2-isopropyl-3-methoxypyrazine, 2,3,4-trichloroanisole, 2,4,6-trichloroanisole, and 2,3,6-trichloroanisole in water samples. This method combined headspace solid-phase microextraction (HS-SPME) with gas chromatography-mass spectrometry and used naphthalene-d(8) as internal standard. A divinylbenzene/carboxen/polydimethylsiloxane fiber exposing at 90°C for 30 min provided effective sample enrichment in HS-SPME. These compounds were separated by a DB-1701MS capillary column and detected in selected ion monitoring mode within 12 min. The method showed a good linearity from 1 to 100 ng L(-1) and detection limits within (0.25-0.61 ng L(-1)) for all compounds. Using naphthalene-d(8) as the internal standard, the intra-day relative standard deviation (RSD) was within (2.6-3.4%), while the inter-day RSD was (3.5-4.9%). Good recoveries were obtained for tap water (80.5-90.6%), river water (81.5-92.4%), and lake water (83.5-95.2%) spiked at 10 ng L(-1). Compared with other methods using HS-SPME for determination of odor compounds in water samples, this present method had more analytes, better precision, and recovery. This method was successfully applied for analysis of earthy-musty odors in water samples from different sources.
一种简单灵敏的方法被开发用于同时分离和测定痕量土腥素类化合物，包括土臭素、2-甲基异冰片、2-异丁基-3-甲氧基吡嗪、2-异丙基-3-甲氧基吡嗪、2,3,4-三氯苯甲醚、2,4,6-三氯苯甲醚和 2,3,6-三氯苯甲醚在水样中。该方法将顶空固相微萃取（HS-SPME）与气相色谱-质谱联用，并使用萘-d(8)作为内标。在 90°C 下暴露 30 分钟的二乙烯基苯/羧基/聚二甲基硅氧烷纤维在 HS-SPME 中提供了有效的样品富集。这些化合物在 DB-1701MS 毛细管柱上分离，并在 12 分钟内以选择离子监测模式检测。该方法在 1 至 100ngL(-1)范围内呈现良好的线性，所有化合物的检测限均在（0.25-0.61ngL(-1)）范围内。使用萘-d(8)作为内标，日内相对标准偏差（RSD）在（2.6-3.4%）范围内，而日间 RSD 在（3.5-4.9%）范围内。自来水（80.5-90.6%）、河水（81.5-92.4%）和湖水（83.5-95.2%）的加标回收率良好，浓度为 10ngL(-1)。与其他使用 HS-SPME 测定水样中气味化合物的方法相比，该方法具有更多的分析物、更好的精密度和回收率。该方法成功应用于不同来源水样中土腥气味的分析。
