Research Of HPLC-MS/MS Analysis Method And Distribution For HBCD

With the rapid development of social industrialization,the pollution problem of brominated flame retardants has been widely concerned by people.Recent years,a great amount of researches of Bromide flame retardants TBBPA,PBDE have been conducted domestically and abroad,but the researchs on new Bromide flame retardants HBCD is limited,and some studies suggest that it is a kind of persistent organic pollutants(POPs),which has the characters of persistence,accumulation,mobility and toxicity.Up to now,there is no standard analytical test methods of HBCD which are used in water,sediments and organismshave have been implemented yet domestically and abroad,in order to study issues about environmental distribution,source and direction and risk assessment of HBCD,sensitive and reliable detection analysis method of HBCD is imperative.Therefore,in this article,HBCD is chosen as the research object,establishing detection methods of three isomers of HBCD in different environmental mediums(water,sediments,organisms),and analysing the distribution characters of three isomers of HBCD in the Huanghai Sea region preliminarily.In this paper,an analysis method by HPLC-MS/MS for detecting HBCD isomers in environmental mediums was established.In liquid phase aspect,the separation degree of HBCD isomers is influenced by different mobile phases,which is discussed.In mass spectrum aspect,the influence in sensitivity by different ion source,detection mode and each parameter of mass spectrum was investigated,and found that three isomers can be completely separated by methanol-0.2%ammonia,and the monitoring method is ESI(—),and the monitoring parent ion is m/z640.6,sub ions are m/z78.9,80.8,238.7,and 13C-HBCD was used as internal standard,so HBCD can be accurately quantified in different environmental media.In this paper,the pre-treatment methods for detection HBCD isomers in environmental mediums(water,sediments,organisms)were developed.In water,the recoveries of HBCD isomers ranged from 84?88%,the detection limit were 0.42,0.52,0.48ng/L;In sediment,the recoveries of HBCD isomers ranged from 76-81%,the detection limit were 0.81,0.87,0.84ng/g;In organisms,the recoveries of HBCD isomers ranged from 65-78%,the detection limits were 1.02,1.06,1.08ng/g.This method is of high sensitivity,good reproducibility,high recovery,low detection limit,which can analysis HBCD isomers in water,sediments,and organisms.The HBCD samples collected from Huanghai Sea,sediment and organisms sample are analysed by the method established in this article.The result suggests that the concentration of HBCD ranged ND-10.08ng/L in the water,ND-14.23ng/g(dry weight)in the sediment,10.86-25.61ng/g(dry weight)in the organism.Analysing the data from detecting preliminarily,and found that HBCD pollution is light in the Huanghai Sea,and is mainly concentrated in Qidong,Yantai,Qingdao which have many production companies,which manifests that the distribution of HBCD is greatly influenced by pollution source.