Study On Pollution And Analysis Of Typical Environmental Endocrine Disrupting In The Baiyang Lake

This thesis consists of three chapters.In CHAPTER ONE, The current state and development of pollution and analysis methods of the typical environmental endocrine disrupting chemicals polybrominated diphenyl ethers and phthalate esters were reviewed. Application of new pretreatment methods and detection methods were summarized.In CHAPER TWO, Dispersive liquid-liquid microextraction (DLLME) is a very simple and rapid method for extraction and preconcentration of polybrominated diphenyl ethers (PBDEs) in water samples, using gas chromatography coupled with the micro-electron capture detector (GC-μECD). In this method, the mixture of chlorobenzene and acetonitrile are injected into samples rapidly, then centrifuging for fifteen minutes at 3000 r/min, after that the organic phase was drawn from the centrifuge tube and evaporated to dryness by nitrogen. The residue was dissolved by 17μL acetone, and 1μL was injected into the GC. Under the optimized conditions, a good linear relationship was obtained in the range of 2.0~250.0μg/L of the analyte with the correlation coefficients of 0.9982~0.9999 and the limits of detection were between 0.17 and 2.50μg/L(S/N=3). The BaiYang Lake water samples were successfully analyzed using the proposed method. The relative recoveries, which had been spiked with different levels, fell in the range of 71.36 %~110.76 % and the relative standard deviations were between 0.99 % and 11.84 %.In CHAPER THREE, A simple method solid-phase microextraction (SPME) coupled with gas chromatography–flame ionization detection (GC-FID) was developed to detect trace levels of phthalate esters (PAEs) in environment water samples. In this method, PDMS fiber was chosen to enrichment the PAEs. The PAEs were extracted for 60 minutes using the chosen fiber under stirring with a magnetic stir bar, after that the fiber was introduced into the GC injector port and the extracts were desorbed at 250℃for 4 minutes for analysis and determination. Under the optimized conditions, 13 phathalate esters (PAEs) can be extracted completely and separated well. The proposed method provides good precision (RSD<10 %) and low limits of detection, ranging from 0.02~0.83μg/L (S/N=3). The water samples collected from Baiyang Lake were successfully analyzed using the proposed method, phthalic acid bis-iso-butyl ester (DIBP), phthalic acid bis-butyl ester (DBP) and phthalic acid bis-2-ethylhexyl ester (DEHP) were detected in all the samples. The recoveries, which had been spiked with different levels (2.5μg/L and 5.0μg/L), fell in the range of 75.3 %~111.0 % and the relative standard deviations were between 2.1 % and 8.0 % (n=3). The results showed that the proposed method would be a valuable for PAEs analysis in environmental water samples.