كاربرد ريز استخراج مايع- مايع پخشي و ريز استخراج فاز مايع با فيبر تو خالي براي پيش تغليظ و اندازه گيري برخي داروهاي مخدر توسط كروماتوگرافي مايع- آشكار ساز آرايه ديودي

چكيده انگليسي :

Application of Dispersive Liquid Liquid Microextraction and Hollow Fiber Liquid Liquid Liquid Microextraction forPreconcentration and Determination of some Narcotic Drugs by Liquid Chromatography Diode Array Detector Maliheh Khalili Boroujeni m boroujeni@ch iut ac ir March 9 2010 Department of Chemistry Isfahan University of Technologhy Isfahan 84156 83111 IranDegree M sc Language FarsiSupervisor Assoc Prof Mohammad Saraji saraji@cc iut ac ir AbstractOpioids main medical use is to relieve acute and chronic pain e g in the treatment of cancer patients andpostoperatively The determination of anaesthetic and analgesic drugs in biological fluids is of major clinicalimportance In this study dispersive liquid liquid microextraction DLLME and hollow fiber based liquid liquid liquid microextraction HF LLLME coupled with reversed phase high performance liquidchromatography diode array detector RP HPLC DAD were applied for simultaneous extraction anddetermination of three narcotic drugs Alfentanil Fentanyl and Sufentanil in biological samples In theDLLME method 2000 L dispersive solution containing 1838 L disperser solvent methanol and 162 Lextraction solvent chloroform was injected rapidly into an aqueous solution contains narcotic drugs with a2500 L syringe Gastight Hamilton Then the mixture was centrifuged at 3500 rpm for 5 min and thesedimented phase was completely transferred to another test tube with conical bottom using a 100 Lsyringe The organic solvent was evaporated by a calm flow of nitrogen gas and the residue was redissolvedin 12 5 L mixture of acetonitrile water 50 50 and 11 L of the solution was injected into HPLC Theeffects of several important parameters influencing the extraction efficiency including type and volume of theextraction solvent type and volume of the disperser solvent concentration of NaOH and salt addition wereinvestigated Optimum conditions were achieved as chloroform as extracting solvent methanol as dispersersolvent extracting solvent volume 162 L volume of disperser solvent 1838 L 0 05 M NaOH without saltaddition Under optimal condition the limits of detection were ranged from 0 4 to 1 9 g L The intra dayand inter day precisions were in the range of 1 2 3 0 and 14 2 15 9 respectively The enrichmentfactors and correlation coffieients ranged from 275 325 and 0 9980 0 9984 respectively The applicability ofthe proposed method was demonstrated by analyzing biological samples plasma and urine In the HF LLLME a layer of the organic phase was impregnated into the pores of a 3 5 cm hollow fiber while the lumen of the fiber was filled with H2SO4 solution as an acceptor solution Then the fiber wasimmersed into 5 ml of aqueous samples and analytes were extracted The effects of several importantparameters influencing the extraction efficiency including organic solvent type concentration of NaOH asdonor solution concentration of H2SO4 as acceptor phase salt addition stirring rate temperature andextraction time were investigated and optimized Under the optimized conditions isoamyl benzoate asorganic solvent 0 5 M NaOH as donor phase 0 05 M H2SO4 as acceptor phase stirring rate of 1200 rpm 20min extraction time no salt addition at 45 oC the limits of detection were ranged from 1 1 to 2 3 g L Theintra day and inter day precisions were in the range of 2 0 4 1 and 3 3 10 1 respectively Theenrichment factors and correlation coefficients ranged from 190 237 and 0 9971 0 9981 respectively Theapplicability of the proposed method was demonstrated by analyzing biological samples plasma and urine Keywords DLLME HF LLLME HPLC DAD Narcotic Drugs Plasma and Urine

خليلي بروجني، مليحه

كاربرد ريز استخراج مايع- مايع پخشي و ريز استخراج فاز مايع با فيبر تو خالي براي پيش تغليظ و اندازه گيري برخي داروهاي مخدر توسط كروماتوگرافي مايع- آشكار ساز آرايه ديودي

داروهاي مخدر , نمونه هاي بيولوژيكي