HS-SPME/GC/MS法测定水中土臭素和2-甲基异崁醇的条件优化
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江苏省科技支撑计划(BE2011797);江苏省卫生厅医学科研项目(H201024)


Determination of GSM and 2-MIB in natural water by headspace solid-phase micro-extraction coupled with gas chromatography/mass spectrometry
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    摘要:

    目的:探索顶空固相微萃取-气相色谱/质谱法(HS-SPME/GC/MS)测定水中嗅味物质土臭素(GSM)和2-甲基异崁醇(2-MIB)的最佳实验条件。方法:应用L32(49)正交表安排顶空固相微萃取-气相色谱/质谱法测定水中嗅味物质时的萃取温度-萃取时间-搅拌子转速-盐浓度-解吸时间和解吸温度并进行实验,优化各项操作参数。结果:顶空固相微萃取-气相色谱/质谱法测定水中嗅味物质的优化后实验条件是:萃取温度和解吸温度分别为65℃和260℃,萃取时间和解吸时间分别是40 min和7 min,搅拌子转速是600 r/min,盐浓度为30%(W/V)。分别测定高低加标样,回收率为91%~107%,检出限(S/N=3)为0.04 ng/L,回收率为91%~104%,检出限(S/N=3)为0.13 ng/L。结论:通过正交实验设计优化实验条件,所建立的分析方法准确-简便-可靠,符合水中嗅味物质的测定要求。

    Abstract:

    Objective:To optimize the conditions for determination of the earthy and musty odors geosmin,2-methylisoborneol (2-MIB) in natural water by headspace solid-phase micro-extraction (SPME) coupled with gas chromatography/mass spectrometry and to establish a proposed method for determining the typical odor compounds in water. Methods:By applying the orthogonal experiment design L32(49) to arrange the determination conditions,several parameters of the extraction and desorption were studied and optimized (such as extraction temperature,desorption temperature,extraction time,ionic strength and rotate-speed),and some other parameters (such as correlation coefficient,limits of detection,RSD and recovery) were applied to evaluate effect of this method. Results:The optimum temperature of extraction and desorption were 65℃ and 260℃,respectively;time of extraction and desorption were 40 min and 7 min,respectively;ionic strength,30%(W/V);rotate-speed,600 rpm. Under the optimized experimental conditions,limits of detection(S/N=3) were 0.04 and 0.42 ng/L for geosmin and MIB,respectively. Calculated calibration curves gave high levels of linearity with correlation coefficient values of 0.9999 for both of geosmin and MIB. Finally,the proposed method was applied to the analysis of seven standard water samples,which were previously analyzed and confirmed free of target analytes. The RSD were 2.75%~3.80% and 4.35%~7.6% for geosmin and 2-MIB,respectively,and the recovery values were 91%~107% and 91%~104% for geosmin and MIB,respectively. Conclusion:The method can be successfully applied to analyze earthy and musty odors in natural water.

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彭世富,丁 震,夏卫文,郑 浩,夏玉婷,陈晓东. HS-SPME/GC/MS法测定水中土臭素和2-甲基异崁醇的条件优化[J].南京医科大学学报(自然科学版),2013,(8):1146-1151

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  • 收稿日期:2012-12-03
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  • 在线发布日期: 2013-07-30
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