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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
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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
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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
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