捕集阱顶空气相色谱/质谱法测定水中的二氯一溴甲烷  

Determination of dichlorobromomethane in water by headspace-trap gas chromatography/mass spectrometry

作　　者：王萍亚[1] 赵华[1] 周勇[1] 许镇坚[1] 戴意飞[1] 张薇英[1] 

机构地区：[1]国家海洋食品质量监督检验中心,浙江舟山316021

出　　处：《色谱》2010年第7期664-667,共4页Chinese Journal of Chromatography

基　　金：浙江省重大科技计划项目(2007C13067);浙江省质量监督系统科研项目(20080244)

摘　　要：建立了捕集阱顶空气相色谱/质谱测定水中二氯一溴甲烷的方法。采用正交实验设计对平衡温度、平衡时间、循环次数3个参数进行了优化,在平衡温度70℃、平衡时间20min、循环次数2次的优化条件下,对水中的二氯一溴甲烷进行测定。结果显示,在0.1～10.0μg/L范围内,二氯一溴甲烷的质量浓度和峰面积呈良好的线性关系,相关系数为0.9991。方法的检出限(S/N=3)为0.03μg/L,定量限(S/N=10)为0.1μg/L,回收率为83.1%～111.3%,相对标准偏差为1.7%～5.2%(n=6)。将该方法应用于水中二氯一溴甲烷的定性定量分析,效果良好。A novel method was developed for the determination of dichlorobromomethane in water using headspace-trap gas chromatography/mass spectrometry （GC/MS）.Three parameters of headspace-trap including thermostatic temperature,time and cycle number were optimized by orthogonal experiment analysis.Dichlorobromomethane in water samples was analyzed under the optimized conditions of 70 ℃ and 20 minutes with the cycle number of two.The results showed that the calibration curve was linear in the range of 0.1-10.0 μg/L,and the correlation coefficient was 0.9991.The detection limit was 0.03 μg/L.The average recovery was 83.1%-111.3% with the relative standard deviation （RSD） not more than 5.2% （n=6）.This method is rapid,sensitive and reproducible for the routine detection of the low concentration of dichlorobromomethane in water.

关 键 词：捕集阱顶空 气相色谱/质谱法 二氯一溴甲烷 水 

分 类 号：O658[理学—分析化学]