Research And Application Of Detection And Analysis Technology Of Endosulfan And Its Derivatives In Marine Ecological Environment

Endosulfan is a broad-spectrum organochlorine insecticide with stomach toxicity and contact toxicity.In view of the environmental durability,bioaccumulation,long-distance migration and high biotoxicity of endosulfan,many countries have banned or severely restricted the use of endosulfan since the 1990s.On March 132019,11 ministries,including the Ministry of Ecological Environment,the Ministry of Agriculture and villages,and the General Administration of Market Supervision,issued an announcement<The ban on the production,circulation,use,import and export of persistent organic pollutants such as Lin Dan>,The production,circulation,use,import and export of Lin Dan and endosulfan are prohibited from March 26 2019.As a new convention controlled persistent organic pollutant,the occurrence form,ecotoxicological effect,migration and transformation behavior of endosulfan in environmental medium has become one of the hotspots of international environmental science research in recent years.Endosulfan is a typical hydrophobic organic compound?HOCs?,with a large octanol/water partition coefficient(K_OW),due to industrial wastewater discharge,agricultural runoff and atmospheric dry and wet deposition,endosulfan enter into the ocean and be accumulated in marine sediments,especially in estuary sediments.Marine sediments are not only the"sink"of endosulfan,but also may become the"source"of secondary pollution.Interstitial water is an important medium for the exchange of endosulfan between sediment and overlying water.The association between dissolved organic matter?DOM?and endosulfan in interstitial water can improve the total solubility of endosulfan.Therefore,this paper through the optimization of the Marine environment of endosulfan and its derivatives in water,sediment and porewater pretreatment and testing conditions,and build a set of Marine ecological environmental samples?water,sediment and interstitial water?,endosulfan and its derivatives in the rapid,accurate and efficient detection method,and applied in China's bohai sea and the jiaozhou bay sea water and sediment state of endosulfan and its derivatives in the research.The main research results are as follows:1.A rapid method for the determination of five endosulfan and its derivatives in seawater by solid phase microextraction?SPME?and gas chromatography?GC?was establelishedThe gas chromatography-electronic capture device?GC-?ECD?was used as the analytical instrument,and the pretreatment and chromatographic conditions were optimized.Under the best experimental conditions,the linear range of the method was0.10¹0.00?g/L,The correlation coefficient was 0.9901⁰.9936,and the detection limit was 0.12¹8.59 ng/L.The standard recovery and relative standard deviation?RSD?of five endosulfonate components in artificial seawater and actual seawater were 89.63%¹10.25%,2.8%⁶.3%and 85.48%¹10.85%,3.1%⁷.6%,respectively,indicating that this method can meet the requirements of rapid detection and analysis of endosulfonate and its derivatives in seawater samples.2.A rapid gas chromatographic method for the determination of five endosulfan and its derivatives in marine sediments was establelishedA rapid method for the determination of endosulfan and its derivatives in marine sediments was established by optimizing the extraction,purification,concentration and analysis conditions of endosulfan and its derivatives in marine sediments.Under optimal experimental conditions,the average recovery and relative standard deviation?RSD?of endosulfan components in blank sediments were 75.71%⁸9.66%,1.7%⁷.4%,and the detection limit of endosulfan and its derivatives was 0.600⁰.703?g/kg.The detection method is used to detect and analyze the soil standard.The detection values of?-endosulfan,?-endosulfan and endosulfan sulfate?standard detection range?were 59.75?g/kg?51.5¹36.0?g/kg?,90.38?g/kg?88.6²33.0?g/kg?and 124.98?g/kg?91.3²41.0?g/kg?,respectively.The results of showed that the method can be used for the determination of endosulfan and its derivatives in sediments of environment.3.A solid phase microextraction-gas chromatographic method for the rapid analysis of five endosulfan and its derivatives in interstitial water was establelishedThe pretreatment and detection methods of endosulfan and its derivatives in seawater continue to be used for the detection of endosulfan and its derivatives in interstitial water.The standard linear range was 0.10¹0.00?g/L,the linear correlation coefficient was0.9902⁰.9981,and the detection limit was 0.10²1.30ng/L.At three standard levels?1.00,5.00 and 10.00?g/L?,the average recoveries of five endosulfan derivatives in artificial seawater were 76.82%¹05.99%,and the relative standard deviations were 2.8%⁸.6%.The method can be used for the detection and analysis of endosulfan and its derivatives in marine sediment interstitial water.4.Using the establelished detection methods to investigate the distribution of endosulfan and derivatives in the seas around Qingdao and the Bohai SeaThe establelished method for the detection and analysis of endosulfan and its derivatives in marine ecological environment was applied to the study of the occurrence of endosulfan and its derivatives in the waters around Qingdao and Bohai Sea.It was found that endosulfan and its derivatives remained in the investigated marine environment,and the content of endosulfan and its derivatives in the environment might pose a potential threat to marine life.The content of endosulfan in the southern end of the Bohai Sea is higher than that in the northern end,and the organic matter content in the sediments of the Bohai Sea is low,which makes it difficult for endosulfan to be adsorbed on the sediment,while the content of endosulfan in intermittent water is slightly higher than that in the sediment.Endosulfan content in the region will be increased in a short period of time,resulting in a certain impact on the marine environment.The concentration of endosulfan and its derivatives in the seawater around Qingdao is low,mainly endosulfan sulfate.The results of three investigation stations in Jiaozhou Bay show that the concentration of endosulfan and its derivatives in the bottom water is higher than that in the surface layer,which may be related to the release of bottom sediments.