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Determination Of Endocrine Disrupting Chemicals NP, OP And BPA In Food

Posted on:2006-06-13Degree:MasterType:Thesis
Country:ChinaCandidate:H HanFull Text:PDF
GTID:2121360182975907Subject:Applied Chemistry
Abstract/Summary:PDF Full Text Request
Alkylphenol ethoxylates(APEOs) are some kinds of non-ion surfactants, whichare widely used in the industrial production. But their metabolites, especiallyNonylphenol(NP) and Octylphenol(OP) have been identified as xenoestrogenicthese years. Another endocrine disrupting chemicals——Bisphenol A(BPA) is alsoan important industrial material usually used in commodity which is very similar toour lives. With large usage of these things, it will be a potential threaten to our health.In this study, the comprehensive analytical methods based on high performanceliquid chromatography and liquid chromatography/electrospray ionization tandemmass spectrometry with solid phase extraction, accelerated solvent extraction andmatrix solid phase dispersion extraction before have been established fordetermination of NP, OP and BPA in food samples (beverage and animal producefood). 4-n-NP has been used as internal standard. The LC separation was performedon a Waters Xterra MS(?)C18 column with a gradient elution system ofmethanol-water as the mobile phase at the flow rate of 0.2mL/min. The DAD tandemfluoresce detector were used for the qualitative and quantitative analyse of HPLCsystem, and triple-quadrupole mass spectrometry analyzer was performed for thequalitative and quantitative analyse of LC-MS/MS system. Satisfactory linearity ofeach compound was obtained in the methods. Intraday (3.0%~5.7%)and interdayvariations(3.8%~5.1%) of the method were all with acceptable ranges.A concentration, enrichment and clean-up with Oasis HLB cartridge wasdeveloped for beverage sample preparation. Recoveries were ranged from 91.08% to103.19% for all compounds at three different spiked levels. The limit of detections(LOD) of the HPLC system were ranged from 7.0 to 28.0 ng/L of DAD detector and1.0 to 2.4 ng/L of fluoresce detector for material drinking water;and from 0.14 to 0.56μg/L of DAD detector and 0.02 to 0.05 μg/L of fluoresce detector for cock. LOD ofthe LC-MS/MS system were ranged from 0.01 to 0.05 ng/L for material drinkingwater;and from 0.4 to 2.4 ng/L for cock. Accelerated solvent extraction combine withNH2 cartridge were developed for meat sample preparation. Recoveries were rangedfrom 88.59% to 101.33% for all compounds at three different spiked levels and theLOD were ranged from 0.9 to 1.4 ng/kg. Preparation of egg and milk samples werebased on matrix solid phase dispersion extraction and solid phase extraction with therecoveries ranged from 79.15 to 98.05% and 82.31 to 102.45 for all compounds atthree different spiked levels respectively. LOD of egg and milk samples were7.6~17.1 ng/kg and 1.9~2.4 ng/kg. The results demonstrated that these methods aresimple, accurate and sensitive for identification and quantification of NP, OP and BPAin food samples.Using the improved methods established in this work, 60 food samples frommarkets in Beijing were determined at last.
Keywords/Search Tags:EDCs, HPLC, LC-MS/MS, SPE, ASE, MSPDE, food
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