固相萃取-气相色谱/质谱选择离子检测法测定水中27种有机农药
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摘要
采用固相萃取(SPE)技术,结合气相色谱/质谱(GC-MS)选择离子检测法(SIM)对水中27种有机农药进行提取、净化、浓缩前处理,实验优选出了分离效果较好的色谱柱VF-1701 ms(30 m×0.25 mm×0.25μm),优化了固相萃取及GC-MS的分析条件,建立了水样中7类27种有机农药的SPE-GC-MS/SIM分析方法。样品中各组分曲线相关系数R2均大于0.9981,检测限为0.015~0.054μg/L,平均加标回收率为72.8%~110.8%,相对标准偏差RSD为5.5%~16%。与传统方法相比,该法无需对有机污染物进行分类处理,可以同时快速测定7类27种有机农药。
A new method was developed for the determination of 27 pesticides in water by using solid phase extraction( SPE) combined with gas chromatography-mass spectrometry( GC-MS) with selected ion monitoring mode( SIM). The chromatographic column VF-1701 ms( 30 m × 0. 25 mm ×0. 25 μm) was preferred by its better separation efficiency,and the optimum conditions of analysis conditions of GC-MS and extraction were studied in detail. Pesticides in the samples were qualitatived and quantitatived in SIM mode,and achieved good results. The correlation coefficients were more than0. 9950,and the detection limits ranged from 0. 015 μg/L to 0. 054 μg/L. The average recoveries were among 72. 8% to 110. 8% with the relative standard deviations of 5. 5% ~ 16%. The method is simple operation, low cost consumption, fast analysis speed, good sensitivity, recovery and reproducibility.
A new method was developed for the determination of 27 pesticides in water by using solid phase extraction( SPE) combined with gas chromatography-mass spectrometry( GC-MS) with selected ion monitoring mode( SIM). The chromatographic column VF-1701 ms( 30 m × 0. 25 mm ×0. 25 μm) was preferred by its better separation efficiency,and the optimum conditions of analysis conditions of GC-MS and extraction were studied in detail. Pesticides in the samples were qualitatived and quantitatived in SIM mode,and achieved good results. The correlation coefficients were more than0. 9950,and the detection limits ranged from 0. 015 μg/L to 0. 054 μg/L. The average recoveries were among 72. 8% to 110. 8% with the relative standard deviations of 5. 5% ~ 16%. The method is simple operation, low cost consumption, fast analysis speed, good sensitivity, recovery and reproducibility.
引文
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[13]EPA 525.2 Determination of organic compounds in dringking water by liquid-solid extraction and capillary columm gas chromatography/mass spectrometry
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[7]LI Bin,XIE Qilai,LIUXinyu,et al.Environ Sci Technol,2014,37(5):102李斌,解启来,刘昕宇,等.环境科学与技术,2014,37(5):102
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[10]LI Jiang,XU Texiu.Pollution Control Technology,2015,28(3):56李江,徐特秀.污染防治技术,2015,28(3):56
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[12]CHENG Zhi,ZHANG Rong,LIU Weihua,et al.Chin J Chromatogr,2014,32(1):57程志,张蓉,刘韦华,等.色谱,2014,32(1):57
[13]EPA 525.2 Determination of organic compounds in dringking water by liquid-solid extraction and capillary columm gas chromatography/mass spectrometry