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  

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

作　　者：杨秦睿 袁蕊[1] 丁文波 YANG Qinrui;YUAN Rui;DING Wenbo(Physical and Chemical Testing Department,Dongcheng Centre for Disease Control and Prevention,Beijing,100050,Chin)

机构地区：[1]北京市东城区疾病预防控制中心理化检验科,北京100050

出　　处：《职业与健康》2023年第24期3359-3363,3368,共6页Occupation and Health

基　　金：北京市东城区卫生科技计划项目(东卫健研[2022]-19)。

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,1.4μm)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1.5~300μg/L、一氯二溴甲烷在0.92~184μg/L、二氯一溴甲烷在0.678~135.6μg/L、其余氯代烃在0.5~100μg/L范围内线性关系良好,相关系数均>0.998,检出限为0.011~0.066μg/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。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,and10 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,1.4μm).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 1.5-300μg/L,chlorodibromomethane in the range of 0.92-184μg/L,chlorobromomethane in the range of 0.678-135.6μg/L,and other halohydrocarbon compounds in the range of 0.5-100μg/L.The correlation coefficients were all>0.998,and the limits of detection were 0.011-0.066μg/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.

关 键 词：卤代烃 静态顶空 气相色谱三重四级杆串联质谱 

分 类 号：R115[医药卫生—公共卫生与预防医学]