全自动顶空固相微萃取-气相色谱-质谱联用测定生活饮用水中痕量臭味物质
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摘要
目的建立全自动顶空固相微萃取-气相色谱-质谱联用同时测定生活饮用水中痕量臭味物质2-甲基异冰片(2-MIB)和土臭素(GSM)的检测方法。方法在选定的顶空固相微萃取条件下,以2-异丁基-3-甲氧基吡嗪为内标,采用气相色谱-质谱选择性离子扫描方式进行定量分析。结果该方法的线性范围为5 ng/L~100 ng/L,相关系数在0.999以上,GSM和2-MIB的检出限(S/N=3)分别为0.05 ng/L和0.15 ng/L,定量限(S/N=10)分别为0.15 ng/L和0.49 ng/L。超纯水加标和水源水加标回收率为88.5%~120%,相对标准偏差RSD为1.2%~13.6%。结论相比2016年生活饮用水臭味物质检测的国家标准方法,本方法具有简便快速、灵敏度高、自动化程度高等优点,检出限更低,更适用于蓝藻暴发时期水样中臭味物质的监测。
Objective To develop a method for the determination of 2-methylisoborneol( 2-MIB) and geosmin( GSM) in water by fully automatic headspace solid phase microextraction( HS-SPME) coupled with gas chromatography-mass spectrometry( GC-MS). Methods Under the selected extraction conditions,with 2-isobutyl-3-methoxypyrazine( IBMP) as the internal standard. Quantitative analysis was performed by gas chromatography-mass spectrometry selective ion scanning.Results The linear range of the method was within 5 ng/L-100 ng/L,the correlation coefficient( r) was above 0. 999,and the detection limits of GSM and 2-MIB( S/N = 3) were 0. 05 ng/L and 0. 15 ng/L,respectively. The limit of quantitation( S/N = 10) was 0. 15 ng/L and 0. 49 ng/L,respectively. The ultra-pure water spiked and source water spiked recoveries ranged from 88. 5% to 120%,and the relative standard deviation( RSD) ranged from 1. 2% to 13. 6%. Conclusion Compared to GB/T 32470—2016,the method was rapid,highly sensitive and automatic,with the detection limit lower than the national standard,so it is much more convenient for monitoring odor compounds in water when blue algae booms.
Objective To develop a method for the determination of 2-methylisoborneol( 2-MIB) and geosmin( GSM) in water by fully automatic headspace solid phase microextraction( HS-SPME) coupled with gas chromatography-mass spectrometry( GC-MS). Methods Under the selected extraction conditions,with 2-isobutyl-3-methoxypyrazine( IBMP) as the internal standard. Quantitative analysis was performed by gas chromatography-mass spectrometry selective ion scanning.Results The linear range of the method was within 5 ng/L-100 ng/L,the correlation coefficient( r) was above 0. 999,and the detection limits of GSM and 2-MIB( S/N = 3) were 0. 05 ng/L and 0. 15 ng/L,respectively. The limit of quantitation( S/N = 10) was 0. 15 ng/L and 0. 49 ng/L,respectively. The ultra-pure water spiked and source water spiked recoveries ranged from 88. 5% to 120%,and the relative standard deviation( RSD) ranged from 1. 2% to 13. 6%. Conclusion Compared to GB/T 32470—2016,the method was rapid,highly sensitive and automatic,with the detection limit lower than the national standard,so it is much more convenient for monitoring odor compounds in water when blue algae booms.
引文
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[9]张振伟,应波,鄂学礼.水中2-甲基异莰醇等3种致嗅物质的顶空固相微萃取-气相色谱-质谱测定法[J].环境与健康杂志,2012,29(5):453-455.
[10]范苓,张晓赟,秦宏兵,等.搅拌棒萃取-热脱附/气质联用法测定水中2-MIB和土臭素[J].环境监测管理与技术,2013,25(6):24-27.
[11]罗添,林少彬.PTV-GC/MS测定饮用水中的土臭素[J].中国卫生与检验杂志,2007,17(12):2227-2228.
[12]马康,张金娜,何雅娟,等.顶空固相微萃取-气质联用测定环境水样中7种痕量土霉味物质[J].分析化学,2011,39(12):1823-1829.
[13]Chen XC,Luo Q,Yuan SG,et al.Simultaneous determination of ten taste and odor compounds in drinking water by solid-phase microextraction combined with gas chromatography-mass spectrometry[J].J Environ Sci,2013,25(11):2313-2323.
[14]Saito K,Okamura K,Kataoka H.Determination of musty odorants,2-methylisoborneol and geosmin,in enviromental water by headspace solid-phase microextraction and gas chromatography-mass spectrometry[J].J Chromatogr A,2008,1186(1-2):434-437.
[15]Peng SF,Ding Z,Xia WW,et al.Orthogonal Design Study on Factors Affecting the Determination of Common Odors in Water Samples by Headspace Solid-Phase Microextraction Coupled to GC/MS[J].J Anal Methods Chem,2013,doi:10.1155/2013/340658.
[2]宼立娟,梁春实,魏树龙,等.固相微萃取-气相色谱-质谱联用测定水中痕量2-甲基异冰片和土臭素[J].分析化学,2011,39(12):1932-1933.
[3]Ding Z,Peng SF,Xia WW,et al.Analysis of Five Earthy-Musty Odorants in Enviromental Water by HS-SPME/GC-MS[J].Int J Anal Chem,2014,doi:10.1155/2014/697260.
[4]彭世富,丁震,陈晓东.水中致嗅物质检测方法研究的进展[J].江苏预防医学,2012,23(4):46-56.
[5]徐娜,刘静,路凤.饮用水中土臭素和二甲基异冰片的分析方法研究进展[J].山东师范大学学报,2010,25(3):107-109.
[6]李宁,安裕敏,张君方.饮用水中土臭素和二甲基异冰片检测方法[J].环保科技,2014,20(2):39-43.
[7]马晓雁,高乃云,李青松,等.饮用水中异嗅物质-土臭素及二甲基异冰片的测定方法[J].环境污染与防治,2006,28(8):631-635.
[8]成建国,刘开颖,白敏冬,等.顶空固相微萃取-气相色谱-质谱联用测定饮用水中的2-甲基异莰醇和土臭素[J].色谱,2015,33(12):1287-1293.
[9]张振伟,应波,鄂学礼.水中2-甲基异莰醇等3种致嗅物质的顶空固相微萃取-气相色谱-质谱测定法[J].环境与健康杂志,2012,29(5):453-455.
[10]范苓,张晓赟,秦宏兵,等.搅拌棒萃取-热脱附/气质联用法测定水中2-MIB和土臭素[J].环境监测管理与技术,2013,25(6):24-27.
[11]罗添,林少彬.PTV-GC/MS测定饮用水中的土臭素[J].中国卫生与检验杂志,2007,17(12):2227-2228.
[12]马康,张金娜,何雅娟,等.顶空固相微萃取-气质联用测定环境水样中7种痕量土霉味物质[J].分析化学,2011,39(12):1823-1829.
[13]Chen XC,Luo Q,Yuan SG,et al.Simultaneous determination of ten taste and odor compounds in drinking water by solid-phase microextraction combined with gas chromatography-mass spectrometry[J].J Environ Sci,2013,25(11):2313-2323.
[14]Saito K,Okamura K,Kataoka H.Determination of musty odorants,2-methylisoborneol and geosmin,in enviromental water by headspace solid-phase microextraction and gas chromatography-mass spectrometry[J].J Chromatogr A,2008,1186(1-2):434-437.
[15]Peng SF,Ding Z,Xia WW,et al.Orthogonal Design Study on Factors Affecting the Determination of Common Odors in Water Samples by Headspace Solid-Phase Microextraction Coupled to GC/MS[J].J Anal Methods Chem,2013,doi:10.1155/2013/340658.