引用本文:孙红梅,朱玉梅,周军.HS/SPME-GC/MS/MS法测定水中痕量2-甲基异莰醇和土臭素[J].环境监控与预警,2017,9(6):40-44
SUN Hong mei, ZHU Yu mei,ZHOU Jun.Determination of Trace 2 MIB and GSM in Water by HS/SPME GC/MS/MS[J].Environmental Monitoring and Forewarning,2017,9(6):40-44
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HS/SPME-GC/MS/MS法测定水中痕量2-甲基异莰醇和土臭素
孙红梅,朱玉梅,周军
盐城市环境监测中心站,江苏 盐城 224002
摘要:
建立了测定水中痕量2-甲基异莰醇(2-MIB)和土臭素(GSM)的顶空固相微萃取-气相色谱/二级质谱联用法(HS/SPME-GC/MS/MS),并对HS/SPME条件进行优化。优化后的方法2-MIB和GSM在1.00~50.0 ng/L范围内,线性良好(r≥0.999 4),RSD分别为7.36%和7.75%,方法检出限分别为0.226和0.239 ng/L,加标回收率分别为87.0%~97.0%和85.2%~112%。结果表明,所建立的方法操作简便、准确度高、重现性好、灵敏度高,无需有机溶剂,适用于水中痕量2-MIB和GSM的测定。
关键词:  顶空固相微萃取  气相色谱/二级质谱  2-甲基异莰醇  土臭素  正交试验
DOI:
分类号:O657.7+1;X832
文献标识码:B
基金项目:
Determination of Trace 2 MIB and GSM in Water by HS/SPME GC/MS/MS
SUN Hongmei, ZHU Yumei,ZHOU Jun
Environmental Monitoring Station of Yancheng, Yancheng,Jiangsu 224002,China
Abstract:
The method of determination of trace 2 MIB and GSM in water was established by headspace solid phase micro extraction (HS/SPME) coupled with gas chromatography/tandem mass spectrometry, and the conditions of HS/SPME were optimized. After the instrument conditions were optimized, the linear relationship between peak area and concentration of 2 MIB and GSM was good enough (r≥0.999 4) from 1.00 to 50.0 ng/L. When the standard sample of 1.0 ng/L was determined 7 times in parallel, the RSDs of 2 MIB and GSM were 7.36% and 7.75% respectively. Their detection limits were 0.226 and 0.239 ng/L, and their quantification limits were 0.904 and 0.956 ng/L, respectively. Two actual water samples were determined and spiked with 2.00 and 20.0 ng/L respectively, and the recovery rates of 2 MIB and GSM were 87.0%~97.0% and 85.2%~112%. The result shows that the proposed method is easily operational, highly accurate, well reproducible, highly sensitive and no need of organic solvents. And it is suitable for the determination of trace 2 MIB and GSM in water.
Key words:  Headspace solid phase micro extraction  Gas chromatography/Tandem mass spectrometry  2 Methylisoborneol (2-MIB)  Geosmin (GSM)  Orthogonal test