仪器参数对气相色谱—质谱法测定多溴联苯的影响  

Influence of Instrument Parameters on the Determination of Polybrominated Biphenyls by Gas Chromatography-Mass Spectrometry

作　　者：吉义平 卢显鹏 宋洲 周宇齐 钟旭 罗火焰 Ji Yiping;Lu Xianpeng;Song Zhou;Zhou Yuqi;Zhong Xu;Luo Huoyan(Hubei Province Geological Experimental Testing Center,Wuhan,Hubei 430034;Hubei Huaxiang Geological Environmental Testing Technology Co.,Ltd.,Wuhan,Hubei 430015;Hubei Key Laboratory of Resources and Eco-environment Geology,Wuhan,Hubei 430034)

机构地区：[1]湖北省地质实验测试中心,湖北武汉430034 [2]湖北华祥地质环境检测科技有限公司,湖北武汉430015 [3]资源与生态环境地质湖北省重点实验室,湖北武汉430034

出　　处：《资源环境与工程》2023年第3期365-371,共7页Resources Environment & Engineering

基　　金：湖北典型水生态环境监测关键技术研究与应用(KJ2021-18、KJ2022-36);土壤中溴代阻燃剂多溴联苯和多溴二苯醚的检测方法研究(CSZXKJ-202114)。

摘　　要：多溴联苯的测定大多采用气相色谱—质谱法,仪器参数是影响其准确测定的关键因素之一。在以十氯联苯(PCB209)为内标的条件下,针对气相色谱—质谱法测定多溴联苯(尤其是高溴代组分)过程中响应低和稳定性差的问题,对仪器参数包括色谱条件、质谱条件和维护保养条件等进行了系统研究。结果表明,在进样口温度为300℃,色谱柱初温为100℃,升温速率为35℃/min的条件下,10种多溴联苯经DB-5HT柱(15 m×0.25 mm×0.1μm)分离可获得良好的效果;在离子源温度为320℃的条件下,以选择离子监测模式可获得良好的响应;通过定期维护衬管、分流平板和离子源可获得良好的响应稳定性,7次重复测量多溴联苯响应比的相对标准偏差为1.65%~5.24%。多溴联苯测定响应低和稳定性差的问题得到有效改善,可为多溴联苯(尤其是高溴代组分)的准确测定提供技术支撑。The determination of polybrominated biphenyls(PBBs)is mostly carried out by gas chromatography-mass spectrometry(GC-MS),and instrument parameters are one of the key factors affecting its accurate determination.Under the condition of using decachlorobiphenyl(PCB209)as the internal standard,aiming at the problems of low response and poor stability in the determination of PBBs,especially the high brominated components by GC-MS,the instrument parameters including chromatographic conditions,mass spectrometry conditions and maintenance conditions were systematically studied.The results showed that under the conditions of sample inlet temperature of 300℃,initial column temperature of 100℃,and heating rate of 35℃/min,ten PBBs were subjected to DB-5HT(15 m×0.25 mm×0.1μm)and good results can be obtained by separation.Under the condition that the temperature of the ion source is 320℃,a good response can be obtained by selecting ion monitoring mode.Good response stability can be achieved through regular maintenance of liner,splitter plate and ion source.The relative standard deviation of response ratio of PBBs for seven repeated test is 1.65%-5.24%.The problems of low response and poor stability in the determination of PBBs have been effectively improved,providing technical support for its pollution prevention.

关 键 词：多溴联苯 气相色谱—质谱法 色谱条件 质谱条件 维护保养条件 

分 类 号：O657.63[理学—分析化学]