顶空固相微萃取-气相色谱-质谱联用法测定土壤中甲基叔丁基醚  

Determination of methyl tert-butyl ether in soil by HS-SPME and GC-MS

作　　者：刘艳茹[1] 梅勇[1] 宋世震[1] 张瑞[1] 代浩[1] 吴宇伉 

机构地区：[1]武汉科技大学医学院公共卫生学院,湖北武汉430065

出　　处：《中国卫生检验杂志》2015年第12期1913-1915,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立顶空固相微萃取-气相色谱-质谱联用法测定土壤中甲基叔丁基醚,并将建立的方法应用到来自不同地区的83份被污染土壤样品的检测中。方法采用顶空固相微萃取富集土壤中的甲基叔丁基醚,后经气相色谱-质谱联用仪进行检测,选择离子监测模式检测碎片离子(m/z=73、57),对萃取时间、萃取温度、盐溶液、分流比以及是否添加搅拌子等条件进行了优化。结果在萃取时间为30 min、萃取温度为35℃、添加5 ml饱和Na Cl溶液、分流比为5∶1的条件下,本方法的线性范围为0.007 5μg/kg^5.000 0μg/kg,最低检出限为0.007 5μg/kg,相关系数(r)为0.999 6,基质加标回收率为84.5%~120.0%,相对标准偏差(RSD)<10%,83份土壤样品中MTBE的含量为0.025μg/kg^0.072μg/kg。结论顶空固相微萃取-气相色谱-质谱联用法灵敏度高、准确度好、操作简便,对土壤样品的检测取得了满意的结果,该方法适用于土壤中痕量MTBE的分析。Objective To establish a method for the determination of methyl tert- butyl ether（ MTBE） in soil by headspace solid- phase microextraction gas chromatography- mass spectrometry（ GC- MS）,and to use it to detect 83 polluted soil samples from different regions. Methods MTBE was gathered by HS- SPME） and determined by GC- MS. To select ion monitoring mode for the detection of fragments ion（ m / z = 73,57）. Some significant variables such as extraction time,extraction temperature,salt concentration,split ratio and add stirring bar were optimized. Relusts Under the suitable conditions of 30 min for extraction,35 ℃ for extraction,5 ml for Na Cl and 5∶1 for split ratio,the calibration linear range for MTBE was among 0. 007 5 μg / kg-5. 000 0 μg / kg,the method detection limit was 0. 007 5 μg / kg and the correlation coefficient was 0. 999 6,the mean recovery values ranged from 84. 5% to 120. 0% and the relative standard deviation（ RSD） was less than 10%. The concentration of MTBE in 83 soil samples was of 0. 025 μg / kg- 0. 072 μg / kg. Conclusion The combination of HS- SPME and GC- MS has advantages of high sensitivity,good accuracy and easy operation. The detection result of soil samples is satisfactory with this method,which can be used for the detection of race MTBE in soil.

关 键 词：甲基叔丁基醚 顶空固相微萃取 气相色谱-质谱 土壤 

分 类 号：O657.63[理学—分析化学]