顶空-气相色谱-串联质谱法同时测定饮用水中8种挥发性卤代烃类有机物
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(佛山市南海区疾病预防控制中心,广东 佛山 528200)

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兰红军 男 主管技师 研究方向为理化检验E-mail:359820312@qq.com

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佛山市南海区“十三五”重点专科(特色专科)建设项目


Simultaneous determination of eight volatile halogenated hydrocarbons in drinking water by headspace-gas chromatography-tandem mass spectrometry
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(Nanhai Center for Disease Prevention and Control, Guangdong Foshan 528200,China)

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    摘要:

    目的 建立同时测定饮用水中8种挥发性卤代烃有机物的顶空-气相色谱-串联质谱(GC-MS/MS)法。方法 准确移取10 ml水样于20 ml顶空瓶中,加入1.0 g NaCl,55 ℃平衡30 min,进入GC-MS/MS进行分析。样品经毛细管柱HP-5MS(30 m×0.25 mm,0.25 μm)分离,采用多反应监测(MRM)模式进行测定,离子峰面积定量,保留时间及特征离子对的丰度比定性。结果 方法线性相关系数(r)为0.999 0~0.999 7,相对标准偏差(RSD)为1.6%~5.2%,加标回收率为85.0%~98.0%(n=6),检出限为0.005 1~0.064 μg/L。结论 本方法具有灵敏度高、精密度好、快速、简便、准确性高等特点,适用于饮用水中的8种挥发性卤代烃准确检测。

    Abstract:

    Objective To establish a method for the simultaneous determination of eight volatile halogenated hydrocarbons in drinking water by headspace-gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods 10 ml of water sample was accurately transferred to a 20 ml headspace vial and 1.0 g NaCl was added, the mixture was equilibrated at 55 ℃ for 30 min, then analyzed by GC-MS/MS. The samples were separated by capillary column HP-5MS(30 m×0.25 mm,0.25 μm)and determined by multi-reaction monitoring (MRM) mode. The quantitative ion peak area was used for quantification, retention time and abundance ratio of characteristic ion pairs was used for qualitative analysis. Results The linear correlation coefficients (r) were from 0.999 0 to 0.999 7, the relative standard deviation (RSD) were from 1.6% to 5.2%, the spiked recoveries were in the range of 85.0%-98.0% (n=6), and the detection limits were between 0.005 1-0.064 μg/L. Conclusion This method was rapid, simple, precise and sensitive. It was suitable for the accurate detection of 8 volatile halogenated hydrocarbons in drinking water.

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兰红军,吴雪梅,冯耀基,黎少映.顶空-气相色谱-串联质谱法同时测定饮用水中8种挥发性卤代烃类有机物[J].中国食品卫生杂志,2019,31(2):121-125.

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  • 收稿日期:2019-01-30
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  • 在线发布日期: 2019-05-17
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