顶空固相微萃取-气相色谱-三重四极杆质谱法测定饮用水中挥发性卤代烃

摘要/Abstract

摘要： 目的建立顶空固相微萃取-气相色谱-三重四极杆质谱联用法分析饮用水中三氯甲烷、四氯化碳、二氯一溴甲烷、一氯二溴甲烷、三溴甲烷。探索萃取纤维头、萃取时间、萃取温度、离子强度、解吸时间对检测结果的影响。方法使用DVB/CWR/PDMS 80 μm萃取头,取10 mL水样到顶空瓶,加入3.0 g NaCl,35 ℃下萃取15 min后于250 ℃解吸5 min,以50 ∶ 1分流比进入气相色谱质谱联用仪进行分析,在多反应监测模式（multi reaction monitoring,MRM）进行检测,外标法定量。结果本方法的线性相关系数（r）均≥0.999,3个加标水平下的平均回收率为80.1%~107.2%（n=6）,相对标准偏差（RSD）为0.4%~10%。利用本方法对生活饮用水进行测定,三氯甲烷、四氯化碳、二氯一溴甲烷、一氯二溴甲烷被检出。结论该方法简单快捷、准确可靠、灵敏度高,适用于短时间分析生活饮用水中常见挥发性卤代烃。

关键词: 顶空固相微萃取, 质谱, 挥发性卤代烃, 饮用水

Abstract: Objective To establish a headspace solid-phase microextraction gas chromatography-triple quadrupole mass spectrometry method for the analysis of trichloromethane,carbon tetrachloride,dichloromethane,dichloromethane,and tribromomethane in drinking water. Explore the effects of fiber head extraction,extraction time,extraction temperature,ion strength,and desorption time on the detection results. Method Using DVB/CWR/PDMS 80 μm extraction head to take 10 mL of water sample into a headspace bottle and adding 3.0 g of NaCl,extract at 35 ℃ for 15 minutes,desorb at 250 ℃ for 5 minutes,and enter gas chromatography-mass spectrometry for analysis at a 50 ∶ 1 split ratio. Detection was performed in multiple reaction monitoring（MRM） mode,with external standard for quantification. Results The linear correlation coefficients（r） of this method were all ≥0.999, and the average recovery rates at three spiking levels were 80.1%-107.2%（n=6）,with a relative standard deviation（RSD） of 0.4%-10%. Using this method to determine drinking water,trichloromethane,carbon tetrachloride,dichloromethane bromide,and dichlorodibromomethane were detected. Conclusion This method is simple,fast,accurate,reliable,and highly sensitive,and is suitable for short-term analysis of common volatile halogenated hydrocarbons in drinking water.

Key words: Headspace solid-phase microextraction, Mass spectrometry, Volatile halogenated hydrocarbons, Drinking water

中图分类号:

R115

王咏欣, 谢承恩, 刘虹, 洪海燕. 顶空固相微萃取-气相色谱-三重四极杆质谱法测定饮用水中挥发性卤代烃. [J]职业与健康, 2024, 40(5): 620-624.

WANG Yongxin, XIE Chengen, LIU Hong, HONG Haiyan. Determination of volatile halogenated hydrocarbons in drinking water by headspace-solid phase microextraction-gas chromatography-triple quadrupole mass spectrometry. [J]OCCUPATION AND HEALTH, 2024, 40(5): 620-624.

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