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Detection Of Antibiotics In Surfacewater And Mycotoxins In Fruits And Vegetables By Ultra Performance Liquid Chromatography-Mass Spectrometry

Posted on:2020-12-14Degree:MasterType:Thesis
Country:ChinaCandidate:J X ChengFull Text:PDF
GTID:2381330602460707Subject:Chemistry
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Environmental safety and food safety were important to the people's property and life and had received widespread attention.There were many kinds of pollutants in the water environment,and antibiotics as potential environmental pollutants had become a research hotspot.The problem of antibiotic abuse was serious.It had been widely found in various water environments in recent years.The physical and chemical properties of different types of antibiotics were different,resulting in different pretreatment methods and detection methods,greatly improving the difficulty of simultaneously detecting different types of antibiotics.Mycotoxins were mainly found in spoiled foods.A variety of mycotoxins had been shown to be carcinogenic and extremely harmful to humans.Therefore,it was especially important to detect mycotoxins efficiently and accurately.In this study,SPE-UPLC-MS/MS was used for detection of commonly used veterinary antibiotics in surfacewater,QuEChERS-UPLC-MS/MS was used for detection of mycotoxins in apple.The cardinal research results are as follows:1?A method was established for rapid detection of 15 kinds of antibiotics(quinolones,chloramphenicol,tetracycline and sulfonamides)in river water near fish farms by solid-phase extraction and ultra-performance liquid chromatography couple with tandem triple quadrupole mass spectrometry(UPLC-MS/MS).Water samples were taken from 24 sampling sites along rivers in May and August,pH of 500mL volume water samples was adjusted to 4.0 with hydrochloric acid,add 0.5g ethylenediaminetetraacetic acid disodium(Na2EDTA)to removal the interference of variousmetal ions,and the water samples were enriched and cleaned by HLB solid-phase extraction column.Seasonal variation of antibiotic concentrations in the river were analyzed by measuring river antibiotic concentration data.To explore the source of antibiotics from the fish ponds nearby,antibiotic concentration data which was investigated in the sediment,fish feed and fish revealed a direct relationship between the main antibiotics and fish farms along the rivers.Risk quotient method(RQ)was used to assess the risk of common veterinary antibiotics in the local ecosystem.2?To establish a neoterio method detecting mycotoxins in jujube and apple by the ultra-high performance liquid chromatography-tandem mass spectrometry.Development of an apple matrix toxin pretreatment method based on a relatively simple pre-treatment method of jujube.The sample was extracted by sonication with 2%formic acid in acetonitrile and 0.5 g NaCl,2.0 g anhydrous magnesium sulfate to remove water,0.4 g PSA adsorbs impurities.15 mycotoxins in apple were separated on a CORTECS C18 column and dectected by multiple reaction monitoring ion model(MRM).The calibration curves of 15 mycotoxins showed good linearity with correlation coefficient more than 0.990.The detection limits were 0.01-100?g/kg.The spiked recoveries of four kinds of toxins from blank matri were between 73.2%and 114.3%,with relative standard deviations of 0.5%-8.6%,which could meet the detection requirements of mycotoxin in apple.At the same time,ToxTree software and T.E.S.T.software were used for risk assessment of six alternaria mycotoxins,the permitted dailyexposures(PDE)of adults for six types of toxins(3.9?67.7?g/d)were obtained based on the calculation of the toxicological software theory.
Keywords/Search Tags:solid-phase extraction, QuEChERS, ultra-high performance liquid chromatography-tandem mass spectrometry, antibiotics, mycotoxins
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