Development Of Solid Phase Sobent-Based Extraction Combined With Liquid Chromatography-Mass Spectrometry For Analysis Of Psychoactive Pharmaceuticals In Environmental Samples

There are many psychotropic drugs in environmental samples with extremely low content,and the matrix of different environmental media is very different.It is necessary to construct sensitive,reliable and simple analytical methods for a variety of psychotropic drugs based on different environmental media.The thesis developed analytical methods for psychotropic drugs in a variety of environmental media(surface water,sediment and aquatic organisms),based on solid-phase sorbent,isotope dilution,and liquid chromatography-mass spectrometry.The proposed method was applied to the analysis of psychotropic drugs in real samples.The occurence of psychotropic drugs in surface water,sediments and wild fish in Wuhan(East Lake,Yangtze River and Han River)was preliminarily explored.The residual levels of psychotropic drugs in aquatic muscle tissue samples in Wuhan were investigated.1.A magnetic solid phase extraction(MSPE)-isotope dilution-UHPLC-MS/MS method was developed for the detemination of antidepressants in various aquatic products muscle tissue.Isotope dilution method and snakehead muscle tissue basedmatrix matched internal standard method were applied for quantitation.In snakehead muscle tissue,the absolute matrix effects of analytes were in the range of 95.4%-105.5%,and the accuracies were in 91.6%-103.6% with RSDs ≤ 7.4%.The accuracies of the method applied in various aquatic products muscle tissue were 84.0%-112.7%,and the lower limits of quantification were 0.002-1.2 ng/g(w.w.).The snakehead drugexposure experiment showed that the target analytes exposed at environmental concentration level had the potential of bioconcentation in sneakehead muscle tissue with different degree.Four drug residues were detected from the muscle tissue samples of 12 aquatic species(37 samples in total).Diphenhydramine and venlafaxine were the most dominant contaminants.2.A PEP-PAN@PSF thin-film microextraction(TFME)combined with UHPLCMS/MS method was proposed for the analysis of various psychotropic drugs in surface water samples.A UHPLC-MS/MS method for the analysis of 47 psychotropic drugs were establiesd.A PEP-PAN@PSF TFME was developed for simutanlously high efficiency extraction of 47 psychotropic drugs.Using isotope dilution method and matrix-matched internal standard method as quantitative methods,the intra-day and inter-day accuracies of 47 analytes at three concentration levels in purified water ranged from 87.9%-110.3%,and the precision was lower than 15.6%.In the recovery tests of the spiked real surface water,the accuracies of 44 analytes were between 80.0% and125.5%,and the precision was lower than 21.4%.Fifteen anaytes were detected in the surface water samples of the East Lake,the Yangtze River and the Han River at least once,with concentrations up to 169 ng/L.Among them,eight compunds were detected in all surface water samples.3.A PEP-PAN@PSF modified Qu ECh ERS method was developed for the analysis of 42 psychotropic drugs in sediments.In the study,PEP-PAN@PSF TFME was untilized to replace the process of dispersed solid phase extraction in traditional Qu ECh ERS,which improved the treatment efficiency of sediment samples.The relevant parameters affecting the extraction efficiency of the sediment were systematically optimized.The performance of the method was evaluated in real samples.Among 42 analytes,39 analytes showed acceptable accuracies(70%-130%)and precision(≤ 20%)with low detection limits(0.001-1.744 ng/g,d.w.)in various sediments of the Yangtze River,Han River and Donghu Lake.Finally,the method was applied to the analysis of psychotropic drugs in the sediments of the East Lake,the Yangtze River and the Han River in Wuhan(6 sampling points),a total of 18 target analytes were detected(nd-1.5 ng/g,d.w.).4.A solid-liquid extraction comnbined with PEP-PAN@PSF TFME method was developed for the analysis of psychotropic drugs in fish muscle tissue.The parameters affecting the extraction efficiency of solid-liquid extraction on 47 psychotropic drugs was optimized.The highly efficient extraction of various psychoactive drugs from fish samples was successfully realized by ombining with the further purification of TFME.The matrix matched method(grass carp muscle)and isotope dilution method were uesd as quantitative methods.As using grass carp muscle as reference matrix,the method showed acceptable accuracies(88.7%-114.1%)and precisions(RSDs ≤ 16.2%)for 44 target analytes in grass carp muscle.The method was applied to the residue analysis of psychotropic drugs in fish tissue(14 samples)from the Yangtze River,the Donghu Lake and the market,and a total of 11 target residues were detected,and their concentrations were raged from not detectable to 35 ng/g(d.w.).