捕集阱顶空－气相色谱质谱法测定水中二氯一溴甲烷.PDF

《色谱》，2010，28(7):664～667 捕集阱顶空－气相色谱质谱法测定水中二氯一溴甲烷 * 王萍亚，赵华，周勇，许镇坚，戴意飞，张薇英 （国家海洋食品质量监督检验中心，浙江 舟山 316021） 摘要：建立了捕集阱顶空-气相色谱质谱法测定水中二氯一溴甲烷的方法。本研究采用正交实验设计对平衡温度、平衡时间、 循环次数3个参数进行优化，确定优化后条件为平衡温度70℃，平衡时间20 min，循环次数2次，并在优化条件下对水中二氯 一溴甲烷进行测定。结果显示，在0.1 ~ 10.0 μg/L范围内，二氯一溴甲烷浓度和色谱峰面积呈良好的线性关系，相关系数为 0.9991，方法检出限是0.03 μg/L （S/N=3 ），定量限为0.1 μg/L （S/N=10 ），回收率为83.1% ~ 111.3%，相对标准偏差为1.7% ~ 5.2% （n=6 ）。本方法可应用于水中二氯一溴甲烷的定性定量测定，效果良好。 关键词 捕集阱顶空；气相色谱质谱法；二氯一溴甲烷；水 Determination of Dichlorobromomethane in Water by Headspace-trap Gas Chromatography-Mass Spectrometry * WANG Pingya , ZHAO Hua, ZHOU Yong, XU Zhenjian, DAI Yifei, ZHANG Weiying (National Marine Food Quality Supervision and Testing Center, Zhoushan 316021, China) Abstract ：A novel method was developed for the determination of dichlorobromomethane in water by headspace-trap gas chromatography-mass spectrometry （GC-MS ）. Three parameters of headspace-trap including oven temperature, thermostatting time, cycle-index were optimized by orthogonal experiment analysis. Dichlorobromomethane in water samples were analyzed under the optimized condition of 70℃ （oven temperature ）and 20 minutes （thermostatting time ）while the cycle-index was two. Results showed that the calibration graphs of the concentration and the peak area was linear in the rang of 0.15 ~ 10.0 μg/L, and the correlation coeficient was 0.9991.The detection limit was 0.03 μg/L. The average recoveries of standard addition were between 83.1% ~ 111.3% with relative standard deviations（RSDs ）less than 5.2%（n=6 ）. This method is rapid, sensitive and reproducible. It can be used for the routine detection of the low concentration of dichlorobromomethane in water ． Keywords ：Headspace tra