بررسي حذف زيستي برخي داروها و توسعه يك روش استخراجي جديد همراه با كروماتوگرافي مايع با كارايي بالا براي اندازه گيري تركيبات دارويي در نمونه هاي آبي

چكيده انگليسي :

Study of Biodegradability of Some Medicines and Development of a New Extraction Method Combined With HPLC for the Determination of Pharmaceuticals in Water Samples Sanaz Sedghi s sedghi@na iut ac ir April 5 2011 Department of Natural Resources Isfahan University of Technologhy Isfahan 84156 83111 IranDegree M Sc Language FarsiSupervisor Assoc Prof Mohammad Saraji saraji@cc iut ac ir AbstractThe first part of this research is dedicated to the biodegradability of 5 pharmaceuticals ampicillin cephalexin cefazolin ceftazidime and acetaminophen Closed bottle test CBT was used as a first simpletest for the assessment of the biodegradability of target compounds The test solution of each drug withconcentration of 3 mg l was prepared with mineral medium and small amounts of microorganisms 0 5 mLinoculums L mineral medium of a population of microbial The mineral solutions are prepared from stocksolutions of appropriate concentrations of mineral components namely potassium and sodium phosphatesplus ammonium chloride calcium chloride magnesium sulphate and iron chloride The blank standard control and suspension solutions were used for determination of degradability of drugs The solutions werehold for a period of 28 days in a closed bottle at constant temperature in the dark or in diffuse light Elimination of them was monitored by high performance liquid chromatography diode array detector Theresults showed that ampicillin cephalexin and aceaminohen were completely eliminated but cefazolin andceftazidime were eliminated 82 and 33 respectively within 28 days In the second part of this thesis solid phase extraction SPE in combination with dispersive liquid liquidmicroextraction DLLME has been developed as a sample pretreatment method with high enrichment factorfor simultaneous extraction and sensitive determination of antidepressant drugs desipramine imipramine amitriptyline and clomipramine in water samples In SPE DLLME antidepressant drugs were extractedfrom aqueous samples by a C18 sorbent 200 mg Then acetic acid 0 1 M methanol solution 15 85 wasused for elution of target compounds from the sorbent and finally the DLLME technique was performed onthe resulting solution Extraction solvent chloroform was added to this solution and was shaked Then anaquous solution cantains 0 05 M NaOH was injected with a syringe Gastight Hamilton rapidly in to theconsiderd solution Finally the mixture was centrifuged and the sedimented phase was completelytransferred to another test tube with conical bottom using a syringe The organic solvent was evaporated by acalm flow of nitrogen gas and the residue was redissolved in 25 L mixture of acetonitrile water 50 50 and20 L of the solution was injected into reversed phase high performance liquid chromatography diode arraydetector RP HPLC DAD The effects of several important parameters influencing the extraction efficiencyincluding flow rate of sample sample volume eluent volume type and volume of the extraction solvent typeand volume of the disperser solvent concentration of NaOH and salt addition were investigated Optimumconditions were achieved as flow rate of sample 4 mL min eluent volume 2 5 mL sample volume 100 mL chloroform as extracting solvent methanol as disperser solvent extracting solvent volume 205 L volume ofdisperser solvent 2 5 mL 0 05 M NaOH without salt addition Under optimal condition the limits ofdetection were ranged from 11 65 ng L The inter day precisions were in the range of 2 3 8 2 Theenrichment factors and correlation coffieients ranged from 1000 1900 and 0 996 0 998 respectively Theproposed method was used for the analysis of river and well water and municipal wastewater samples andsatisfactory results were achieved Keywords Closed Bottle Test DLLME SPE HPLC DAD Pharmaceutical Water samples

صدقي، ساناز

بررسي حذف زيستي برخي داروها و توسعه يك روش استخراجي جديد همراه با كروماتوگرافي مايع با كارايي بالا براي اندازه گيري تركيبات دارويي در نمونه هاي آبي

آزمايش بطري در بسته , استخراج فاز جامد , ريز استخراج مايع-مايع پخشي