آناليزبرخي تركيبات دارويي و زيستي در نمونه هاي ادرار و پلاسماي خون بااستفاده از روش هاي مختلف استخراج فاز جامد با جاذب هاي نانو الياف و پليمرقالب مولكولي و ريز استخراج فاز مايع با فيبرتو خالي با دستگاه طيف سنج تحرك يوني

چكيده انگليسي :

Analysis of some biological compounds in urine and plasma samples using nanofiber and molecular imprinted polymer solid phase extraction and hollow fiber based liquid phase microextraction followed by ion mobility spectrometry Shiva Mirmahdieh Email address Shiva mirmahdieh@yahoo com September 2012 Department of Chemistry Isfahan University of Technology Isfahan 84156 83111 IranSupervisor Professor T Khayamian Email address Taghi@cc iut ac irAdvisor Associated Professor M SarajiDepartment of Chemistry Isfahan University of Technology Isfahan 84156 83111 Iran Tel 98 311 3913248 Fax 98 311 3912350AbstractIn this thesis different sample preparation methods such as packed fiber solid phase extraction PFSPE molecular imprinted solid phase extraction MISPE and Hollow fiber based liquid liquid liquidmicroextraction HF LLLME followed by corona discharge ion mobility spectrometry CD IMS were used forthe determination of biological and pharmaceutical compounds In the first part Analysis of testosterone in urine sample was accomplished using CD IMS Molecular imprintedpolymer was used for the extraction and pre concentration of testosterone Under the optimized conditions thelimit of detection was calculated to be 0 9 ng mL The results from obtained the method were also comparedwith the standard method for analysis of testosterone using SPE HPLC technique The results demonstrate theaccuracy of the method In the second work HF LLLME combined with CD IMS was developed for theanalysis of amantadine in human urine and plasma samples All variables affecting the extraction of analytewere optimized The limits of detection were calculated to be 7 2 and 1 6 ng mL for plasma and urine samples respectively In the third part the capability of CD IMS for separation and quantification of sarcosine and L alanine isomers has been evaluated for the first time Variables including carrier gas flow rate injection and celltemperatures were optimized At the optimized conditions the detection limit of sarcosine and L alanine were0 7 and 0 9 g mL respectively Furthermore in this work since ion peak of sarcosine overlaps with methanolpeak a solvent free sample introduction system was developed In the next part HF LLLME followed bycorona discharge ion mobility spectrometry was presented for analysis of dextromethorphan andpseudoephedrine in urine and plasma samples The effects of various parameters on HF LLLME wereoptimized Under the optimized conditions the limits of detection are 0 6 and 0 3 ng mL for dextromethorphan and 8 6 and 4 2 ng mL for pseudoephedrine in plasma and urine samples respectively In the next section electrospun nanofibers from poly methylmethacrylate PMMA and polystyrene PS blend were used as asorbent to extract tramadol from urine and plasma samples and then determined by CD IMS The scanningelectron microscopy SEM images of the PMMA PS nanofibers showed a diameter range of 130 600 nm with asmooth morphology Parameters affecting extraction efficiency were optimized and under the optimizedconditions the detection limits of tramadol were found to be 9 4 and 1 6 ng mL in plasma and urine samples respectively In the last part a second order calibration method Tucker 3 is proposed on CD IMS data Theresults of Tucker 3 were also compared with the PLS N PLS and U PLS models indicating superiority of theTucker 3 model over the others Key words Corona discharge ion mobility spectrometry Molecular imprinted polymer Hollow fiber basedliquid liquid liquid microextraction Electrospun nanofibersIntroductionThe ion mobility spectrometry IMS is a sensitive simple fast and portable analyticaltechnique for the detection of organic compounds at low concentrations 1 The combination

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