职业与健康 ›› 2023, Vol. 39 ›› Issue (24): 3359-3363.

• 论著 • 上一篇    下一篇

水中13种卤代烃的静态顶空-气相色谱-三重四级杆串联质谱测定法

杨秦睿, 袁蕊, 丁文波   

  1. 北京市东城区疾病预防控制中心理化检验科,北京 100050
  • 收稿日期:2023-07-21 修回日期:2023-08-14 出版日期:2023-12-15 发布日期:2026-03-26
  • 作者简介:杨秦睿,女,检验技师,主要从事理化检验工作。
  • 基金资助:
    北京市东城区卫生科技计划项目(东卫健研[2022]-19)

Determination of 13 halohydrocarbon compounds in water by gas chromatography-triple quadrupole tandem mass spectrometry after static-headspace

YANG Qinrui, YUAN Rui, DING Wenbo   

  1. Physical and Chemical Testing Department,Dongcheng Centre for Disease Control and Prevention,Beijing 100050,China
  • Received:2023-07-21 Revised:2023-08-14 Online:2023-12-15 Published:2026-03-26

摘要: 目的 建立水中13种卤代烃静态顶空-气相色谱-三重四级杆串联质谱测定方法。方法 取4.00 g硫酸钠置于顶空瓶中,加入10 mL采集水样,立即密封摇匀。将顶空瓶放入孵化器中,于80 ℃平衡25 min。抽取瓶内气相部分进样,以VF-624MS(30 m×0.25 mm,1.4 μm)柱对目标化合物进行色谱分离,多反应监测模式(multiple reaction monitoring,MRM)下测定13种卤代烃化合物,外标法定量, 结果 1,2-二氯乙烷和三溴甲烷在1.5~300 μg/L、一氯二溴甲烷在0.92~184 μg/L、二氯一溴甲烷在0.678~135.6 μg/L、其余氯代烃在0.5~100 μg/L范围内线性关系良好,相关系数均>0.998,检出限为0.011~0.066 μg/L,加标回收率为68.7%~119.5%,精密度为1.1%~9.2%。结论 所建立的方法具有快速、简单、灵敏度高和精密度好等特点,适用于水中13种卤代烃检测。

关键词: 卤代烃, 静态顶空, 气相色谱三重四级杆串联质谱

Abstract: Objective To establish a method for determination of 13 halohydrocarbon compounds by gas chromatography-triple quadrupole tandem mass spectrometry after static-headspace. Methods 4.00 g sodium sulfate was put into a headspace bottle,and 10 mL water sample was added. After sealing immediately and shaking vigorously,the headspace bottle was placed in the incubator and balanced at 80 ℃ for 25 minutes. Some gas of the bottle was extracted into analyzer,and the target compounds were separated on VF-624MS column(30 m×0.25 mm,1.4 μm). 13 halohydrocarbon compounds were determined with positive ion electrospray multiple reaction monitoring mode(MRM) and external standard method was used for quantification. Results It was shown that the linear relationship was good:1,2-dichloroethane and tribromomethane in the range of 1.5-300 μg/L,chlorodibromomethane in the range of 0.92-184 μg/L,chlorobromomethane in the range of 0.678-135.6 μg/L,and other halohydrocarbon compounds in the range of 0.5-100 μg/L. The correlation coefficients were all >0.998,and the limits of detection were 0.011-0.066 μg/L. The recoveries were 68.7%-119.5%,and the precisions were 1.1%-9.2%. Conclusion This method is rapid,simple,precise and sensitive,and it is suitable for the determination of 13 halohydrocarbon compounds in water.

Key words: Halohydrocarbon compounds, Static-headspace, Gas chromatography-triple quadrupole tandem mass spectrometry

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