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Rapid Determination of Geosmin and 2-MIB in Water by Headspace Solid Phase Microextraction Gas Chromatography-Mass Spectrometry

机译:顶空固相微萃取气相色谱-质谱法快速测定水中的土臭素和2-MIB

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A simple and sensitive technique, headspace solid-phase microextraction (HS-SPME) linked to gas chromatography-mass spectrometry (GC-MS), was developed for the determination of musty odor compounds, geosmin and 2-methylisoborneol. To obtain the highest sensitivity, several parameters of the extraction and desorption procedure were studied and optimized (such as extraction temperature, extraction time, ionic strength, sample volume, desorption temperature and desorption time). The optimum extraction conditions were as follows: extraction temperature 60°C, extraction time 50 min, ionic strength of 0.3 g mL-1 NaCl, sample volume 20 mL, desorption temperature 250°C, desorption time 5 min. The method showed a good linearity from 2 to 1000 ng L-1 with the coefficients of determination 0.999 for geosmin and 0.988 for 2-MIB. It provided detection limits of 0.67 ng L-1 of geosmin and 0.45 ng L-1 of 2-MIB. The relative standard deviations (R. S. D. S) were within 6.8% for geosmin and 4.4% for 2-MIB. Good recoveries were obtained for tap water (2-MIB 103%, GSM 98%) and lake water (2-MIB 94%, GSM 89%) spiked at 10 ng/L. The method is easily operational and suitable for the determination of musty odor compounds in water. Finally, the method was successfully applied to analyze musty odor compounds in tap water and lake water.
机译:开发了一种简单而灵敏的技术,与气相色谱-质谱联用(GC-MS)的顶空固相微萃取(HS-SPME),用于测定发霉的气味化合物,土臭素和2-甲基异冰片醇。为了获得最高的灵敏度,对萃取和脱附过程的几个参数进行了研究和优化(例如萃取温度,萃取时间,离子强度,样品量,脱附温度和脱附时间)。最佳提取条件如下:提取温度60°C,提取时间50 min,离子强度0.3 g mL-1 NaCl,样品量20 mL,解吸温度250°C,解吸时间5 min。该方法在2至1000 ng L-1范围内显示出良好的线性,对土臭素的测定系数为0.999,对于2-MIB的测定系数为0.988。它提供了0.67 ng L-1的土臭素和0.45 ng L-1的2-MIB检测限。土臭素的相对标准偏差(R. S. D. S)在6.8%之内,而2-MIB的相对标准偏差在4.4%之内。加标浓度为10 ng / L的自来水(2-MIB 103%,GSM 98%)和湖水(2-MIB 94%,GSM 89%)获得了良好的回收率。该方法操作简便,适用于测定水中的霉味。最终,该方法成功地用于分析自来水和湖水中的霉味。

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