Establishment And Application Of The HPLC-MS-MS Method Of Perfluorinated Compounds In Environmental Media

Perfluorinated compounds are a kind of organic compounds containing fluorine,which arewidely used in industrial productions and human daily life.They include surfactants,foam fire extinguishing agent,additives,etc.In May,2009,the United Nations Environment Programme of American included perfluorooctanoic acid and its salts in the model of persistent organic pollutants,and proposed a ban on the use of the compounds.As a new type of organic pollutant,it is characterized by persistence,long distance transmission,bioaccumulation,toxicity,etc.It is difficult for biodegradation and photodegradation in the environmental media.At present,it universally exists in the environmental media such as atmosphere,water,sediments,biological samples etc.,bringing crisis to human health and the living environment to a large extent.In order to better understand the concentration level and tendency of perfluorinated compounds in the global media,it is very important to establish a perfect method of quantitative analysis of perfluorinated compounds.Therefore,this thesis chooses 17 perfluorinated compounds as the research objects,establishes the LC/MS/MS method and pretreatment method of perfluorinated compounds in multi medium,and applies them to the detection of the sediments from Shandong Laizhou Bay Area and the sediments from Antarctic lake water,snow water.This thesis further investigates the possible sources of perfluorinated compounds in the Antarctic region.First,this thesis establishes the HPLC-MS/MS method of 17 perfluorinated compounds.Mass spectrometric conditions are selected by negative ion mode and analyzed by selected reaction monitoring mode(SRM),and the parent iron and the daughter ion of target compounds are scanned to find the characteristic ion.qualitative and quantitative ion for PFOA and PFNA is369/218,519/318.The chromatographic conditions are that 10 mmol/L ammonium acetate and methanol are selected as the mobile phases to separate 17 perfluorinated compounds.Second,this thesis establishes the pre-treatment method of environmental media including water,sediment,creature.Solid phase extraction is selected to extract water samples,during the process we select the best eluent.the recoveries of PFCs ranged from73.10~103.26 %.the detection limit were 0.02 ~0.16 ng/L.For the sediment samples,this studyrespectively compares the effects of methanol ultrasonic extraction method,ion pair reagent extraction and alkaline digestion method on the extraction of sediment,and finally chooses alkali digestion method.the recoveries of PFCs ranged from 67.37 % ~ 111.4 %.the detection limit were 0.02~0.05 ng/g.Using the combination of alkaline digestion method and frozen method for the biological samples,which solves the problem of column blockage in the process of solid phase extraction.The method of high sensitivity,good reproducibility,high recovery,low detection limit,has met the requirements of environmental medium.Finally,according to the established method,this thesis detects the sediments from Shandong Bay area of Laizhou,and the results show that 17 perfluorinated compounds are all detected and the detection rate of PFOA is highest.The results of Antarctic peninsula field show the composition feature is ? PFPeA > ? PFHx A > ? PFBA > ? PFHpA.According to the linear relationship between organic carbon and perfluoronic compounds and the relevency of PFOS/PFOA,this thesis preliminary analyzes the possible source of the perfluoronic compounds in Antarctic region.In addition,the lake water and snow water from Antarctic Zhongshan Station are also monitored by this method.