Research On The Determination Of Alkyl Phenol And Bisphenol Compounds

Because of alkyl phenol and bisphenol compounds have a structure similar to the natural estrogen which made their having estrogenic activity, therefore were called phenolic environmental estrogens. Environmental hormones are trace chemicals in the environment, usually enters the organism through the food chain. This process may formation of false hormones which transmitted pseudo-chemical signals and affect hormone levels in organism, and thus interfere with the original mechanism of endocrine caused by endocrine disorders, harm organisms or cause cancer. Therefore, the establishment of a sensitive, efficient, reliable detection of the alkyl phenol and bisphenol compounds of method is particularly important. In this study, high-performance liquid chromatography for the determination of bisphenol A, bisphenol AF, tetrabromobisphenol A, octylphenol,4-phenylphenol and2-4dichloropheno are discussed, the main research contents are as follows:Part1Cloud point extraction for the determination of bisphenol A, bisphenol AF and tetrabromobisphenol A in river water samples by High-Performance Liquid ChromatographyIn this study, cloud point extraction (CPE) was developed to preconcentrate and separation bisphenol A (BPA), bisphenol AF (BPAF) and tetrabromobisphenol A (TBBPA) prior to high-performance liquid chromatography (HPLC) analysis. Alcohol ethoxylate (AEO9) was applied as the extractant and octanol worked as cloud point revulsant and synergic reagent for extraction, which decreased the cloud point temperature (CPT) of AE09from75℃to30℃and assisted the subsequent extraction. The optimum conditions of the proposed method were pH3.0,125μL octanol,0.5%(v/v) Alcohol ethoxylate,8min equilibration time at30℃and5min centrifugation time at3000rpm. Under the optimum conditions, the linear range of BPA, BPAF and TBBPA was from0.05to25mg L-1. The relative standard deviations (RSD, n=5) were1.6-4.7%. The limits of detection (LOD) were in the range of 0.27-0.32μgL-1. The proposed method was successfully applied to the extraction of BPA, BPAF and TBBPA in river water samples.Part2Supramolecular solvent microextraction combined with high-performance liquid chromatography for the determination of synthetic endocrine disrupting compoundsChapter1Determination of bisphenol-A,2,4-dichlorophenol, bisphenol-AF and tetrabromobisphenol-A in liquid foods and their packaging materials by vortex-assisted supramolecular solvent microextraction/High-Performance Liquid ChromatographyA fast microextraction technique termed vortex-assisted supramolecular solvent microextraction (VASUSME) has been developed. The method was based on the microextraction of endocrine disrupting compounds (EDCs), including bisphenol-A (BPA),2,4-dichloropheno (2,4-DCP), bisphenol-AF (BPAF) and tetrabromobisphenol-A (TBBPA) in10ml sample, and then detected by high-performance liquid chromatography (HPLC). The optimum conditions of the proposed method were pH7.0,500μL supramolecular solvent,2min vortex time at3000rpm and5min centrifugation time at3500rpm. Under the optimum conditions, the repeatability of the proposed method was found to be good. The relative standard deviations (RSD, n=5) were3.98%-5.64%. The limits of detection (LOD) were in the range of0.14-0.32ng mL-1. All correlation coefficients of the calibration curves were higher than0.998. Recoveries of the EDCs spiked into liquid foods and their packaging materials samples were in the range of91%to105.1%. The VASSUSME method was successfully applied to the analysis of the BPA,2,4-DCP, BPAF and TBBPA in liquid foods and their packaging materials samples.Chapter2Vortex-assisted supramolecular solvent microextraction combined with high-performance liquid chromatography-fluorescence detector for the fast determination of synthetic endocrine disrupting compounds in waterA simple vortex-assisted supramolecular solvent emulsification microextraction (VASUSEME) was developed for the preconcentration of four synthetic endocrine disrupting compounds (bisphenol-A (BPA),2,4-dichlorophenol (2,4-DCP),4-phenylphenol (4-PP), bisphenol-AF (BPAF)) in water samples prior to high-performance liquid chromatography-fluorescence detector (HPLC-FLD) analysis. The supramolecular solvents (SUPRASs) tested were made up of vesicles of nonoic acid (NoA) dispersed in1-butyl-3-methylimidazolium tetrafluoroborate ([BMIM][BF4])-water. The optimum conditions of the proposed method were pH7.0,400μL supramolecular solvent,1min vortex time at3000rpm and5min centrifugation time at3500rpm. The linear range of BPA,2,4-DCP,4-PP, and BPAF was from0.1to20ng L-1. Compound recoveries were more than95.8%in water matrices. The relative standard deviations (RSD, n=5) were2.1-6.8%. The limits of detection (LOD) were in the range of61.5-103.2ng L-1. The proposed method was successfully applied to the extraction of EDCs in water samples as a fast, efficient, and convenient method.Part3Vortex-assisted hollow-fiber liquid-phase microextraction coupled with high performance liquid chromatography for the determination of three synthetic endocrine disrupting compounds in milkIn this study, a vortex-assisted three-phase hollow fiber liquid-phase microextraction (VA-HF-LPME) coupling with high performance liquid chromatography (HPLC) method was developed for determination of three synthetic endocrine disrupting compounds(EDCs, bisphenol-A (BPA), bisphenol-AF (BPAF) and tetrabromobisphenol-A (TBBPA)) in milk samples. The influencing parameters of VA-HF-LPME sample preparation method, such as organic solvents (acceptor phase), pH of sample solution (donor phase), sample volume, concentration of NaOH, extraction time, and ionic strength were systematically optimized. The instrumental calibration curves of BPA, BPAF and TBBPA show good linear relations (R>0.9988) in the concentration range of0.5-200,0.5-200and1.0-250μg L-1, respectively. The relative standard deviations (RSD, n=5) were1.3-3.7%. The limits of detection (LOD) were in the range of0.16-0.34μg L-1. Vortex provided effective and mild mixing of the sample solution and increased the contact between analytes and boundary layers of the hollow fibre, thereby enhancing mass transfer rate and leading to high extraction efficiency of the·target analytes. The proposed method was successfully applied to the extraction of EDCs in milk samples.