5844

5459

كارشناسي ارشد

شيمي تجزيه

اصفهان: دانشگاه صنعتي اصفهان، دانشكده شيمي

1389

سيزده،74ص.: مصور،جدول،نمودار

ص.ع.به فارسي و انگليسي

محمد سراجي، محمد تقي جعفري

10/2/90

تقي خياميان، بهزاد رضايي

شيمي

ID5459

به فارسي و انگليسي: قابل رويت در نسخه ديجيتالي

Application of hollow fiber based liquid liquid liquid microextraction with in syringe derivatization for the determination of desipramine in biological samples by gas chromatography nitrogen phosphorus detector Narges Mehrafza n mehrafza@ch iut ac ir October 27 2010 Department of Chemistry Isfahan University of Technologhy Isfahan 84156 83111 Iran Degree M sc Language Farsi Supervisor Dr Mohammad Saraji saraji@cc iut ac ir Dr Mohammad Taghi Jafari jafari@cc iut ac ir Abstract Liquid phase microextraction based on hollow fiber is one of the liquid phase microextraction techniques that have been considered in recent years In three phase hollow fiber an aqueous acceptor phase is used for the extraction of analytes from sample solution that can be injected only to high performance liquid chromatography and capillary electrophoresis So for extraction of compounds before analysis with gas chromatography a two phase hollow fiber is used In this study instead of two phase a three phase HF LPME was used for the extraction and preconcentration of desipramine before analysis with gas chromatography Methanol was used as an acceptor phase instead of aqueous phase So this new three phase method can be used for the extraction of analytes before inject to gas chromatography Determination of desipramine in biological samples such as plasma and urine was performed using in syringe derivatization and followed by gas chromatography nitrogen phosphorus detector In the hollow fiber liquid liquid liquid microextraction the lumen of hollow fiber was filled with methanol as an acceptor phase Then a layer of organic phase n dodecane was impregnated into the pores of an 8 mm porous hollow fiber The fiber was then immersed into 3 ml of a basic aqueous sample Due to its low cost the hollow fiber was disposed after a single extraction that eliminated the possibility of carry over effects After extraction desipramine was derivatized using acetic anhydride as derivatization reagent Then the derivatized analyte was injected to the GC NPD Derivatization reaction was performed using 0 6 L of acetic anhydride at room temperature for 2 min The effect of parameters influencing the extraction efficiency such as organic solvent type concentration of sodium hydroxide in donor solution sample stirring rate salt addition extraction temperature and extraction time were studied The best extraction efficiency was obtained using 0 05 M sodium hydroxide as donor phase stirring rate of 900 rpm 25 min extraction time no salt addition at room temperature The intra day and inter day relative standard deviation of the method were 2 6 and 7 7 respectively The enrichment factor limit of detection and correlation coefficients were 90 0 02 g L and 0 9986 respectively Key Words Hollow fiber based liquid liquid liquid Microextraction Gas chromatography Nitrogen phosphorus detection Desipramine Acetic anhydride Biological samples

محمد سراجي، محمد تقي جعفري

تقي خياميان، بهزاد رضايي