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Determination Of 20 Perfluorinated Alkyl Substances In Honey By High Performance Liquid Chromatography-tandem Mass Spectrometry

Posted on:2018-07-04Degree:MasterType:Thesis
Country:ChinaCandidate:S LiFull Text:PDF
GTID:2321330512990589Subject:Food engineering
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Perfluorinated alkyl substances(PFASs)is a new kind of persistent organic pollutants,which is artificially synthesized and composed of different lengths of hydrophobic alkyl carbon chains and hydrophilic end groups,with strong stability,excellent chemical inertness and heat resistance and other excellent performance.Hydrogen atoms in hydrophobic alkyl carbon chains are all replaced by fluorine atoms,which Forms a C-F bond with extremely high chemical energy(about 110 kcal/mol).In the 1950 s,It was used surfactants,catalysts,lubricants,insecticides and as an intermediate for synthetic drugs,fluororubber,and resin on a wide range.PFASs are difficult to be metabolized,hydrolyzed,photolyzed,biodegraded,and can accumulate in the body with the passage of time.The accumulation of PFASs in organisms is higher than the hundreds of thousands of times that of persistent organic pollutants such as organochlorine and dioxin.A large number of studies have found that perfluorooctanoic acid(PFOA)and perfluorooctane sulfonate(PFOS)with neurotoxicity,liver toxicity,cardiovascular toxicity,thyroid toxicity and reproductive toxicity.At present,domestic and foreign scholars have detected PFASs in the aquatic products,animal liver,eggs,milk,and breast milk,and dietary intake had become one of the sources of PFASs in the human body.In this paper,the rapid determination of PFASs in honey by liquid chromatography-tandem mass spectrometry was carried out.The main research contents are as follows.A sensitive method for simultaneous determination of 20 perfluorinated alkyl substances(PFASs)in honey was developed by Qu ECh ERS-high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were extracted by acetonitrile with 1.5%(v/v)formic acid,and purified by C18 and N-propylethylenediamine(PSA).The separation of the 20 PFASs was performed on an Atlantis T3 C18 column using gradient elution with methanol containing 5 mmol/L ammonium acetate and 5 mmol/L ammonium acetate as mobile phase within 16 min.The PFASs were analyzed under the multiple reaction monitoring(MRM)mode with negative electrospray ionization(ESI-).Under the optimal conditions,the isotope internal standard method was used to quantify the contents of the 20 PFASs.The calibration curves were acquired in the concentration range of0.2-10 ?g/L with correlation coefficients(r)greater than 0.99.The limits of detection(LODs)and limits of quantitation(LOQs)were ranged from 0.04 to 0.10 ?g/kg and 0.10 to 0.20 ?g/kg,respectively.The recoveries of the 20 PFASs spiked in blank honey samples were between 72.6% and 113.0% with relative standard derivations(RSD)of 0.4%-15.9%(n=6).The developed method is rapid,efficient and accurate,and suitable for simultaneous analysis of the 20 PFASs in honey samples.
Keywords/Search Tags:high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS), QuEChERS, perfluorinated alkyl substances(PFASs), honey
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