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3 protocols using ammonia solution

1

Khat Waste Extraction and Characterization

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Khat waste was collected from Obsa Special Khat Shop, Addis Ababa, Ethiopia and cut into small pieces. Formic acid (98%) (Central Drug House (P) Ltd. New Delhi, India), acetone and sodium hydroxide 97% (HiMedia, Mumbai, India), acetic acid 99.8% (Riedel-de Haën), sulfuric acid 97% (BDH, England), copper sulfate pentahydrate 98.5%, n-hexane 99% and zinc chloride (LOBA CHEMIE-Laboratory, India), toluene (Fisher Scientific, UK), potassium iodide (Reagent chemical services Ltd Runcorn, Cheshire), ammonium oxalate 99.5% (UNI-Chem, Chemical Reagents), iodine 99%, methanol 99.9%, and ammonia solution 28% (CARLO ERBA reagents, France), ethanol absolute (Fisher Scientific, UK), hydrogen peroxide 50% (Awash Melkasa, Ethiopia), diclofenac sodium (Healthcare Limited PLC, India), triethanolamine (Fischer Chem Alert Guide, USA), potassium dihydrogen phosphate (Sörensen, Leuren, Denmark), disodium hydrogen phosphate (Fizmerk chemicals, India), sodium chloride (Oxford Laboratory, Mumbai, India), sodium carboxymethylcellulose (FMC Corporation, USA), and propylene glycol (Research-lab fine Chem. Industries, India) were used as received.
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2

Quantification of Sulfonamide Residues

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Ammonia solution (30%), acetic acid (99.5%), n-hexane (95%), ammonium acetate (98%), were purchased from Carlo Erba Reagents (Rodano, Italy). Chloroform and acetone (analytical grade) were obtained from Panreac (Barcelona, Spain). Water, acetonitrile and methanol of HPLC grade were purchased from Baker (Deventer, Holland). The 0.02 M acetate buffer solution, used as solution (A) for HPLC mobile phase, was prepared by dissolving 1.54 g of ammonium acetate in water. The pH value was adjusted to 4.50±0.02 with acetic acid. Standards of SAs [sulfadiazine (SDA) 99.3%, sulfathiazole (STZ) 99.9%, sulfapyridine (SP) 99.7%, sulfamerazine (SM) 98.8%, sulfamethazine (SMZ) 99.8%, sulfamethoxipyridazine (SMP) 99.7%, sulfachloropyridazine (SCP) 99.4%, sulfamonomethoxine (SMM) 98%, sulfamethoxazole (SMX) 99.9%, sulfadoxine (SDO) 99.8%, sulfaphenazole (SNZ) 99%, sulfadimethoxine (SDM) 99.8% and sulfaquinoxaline (SQX) 96%] were supplied by Sigma-Aldrich (Steinheim, Germany).
Working standards at concentration of 0.25-0.5-1.0-2.0-4.0 mg/L were prepared by appropriate dilution in mobile phase to make calibrations curves for the detection of SAs in meat. A feed sample fortified at five concentrations (0.2, 1.0, 5.0, 10.0 and 20.0 mg/kg) with standard solutions of SAs before the extraction was used to obtain the calibration curve for the analysis of SAs in feed.
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3

Synthesizing Pharmaceutical Compounds

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All the chemicals employed were reagent grade or higher in quality. OFL, zeolite Y in sodium form, sepiolite powder, titanium (IV) tetraisopropoxide (97% v/v), and 2-propanol (99.5% v/v) were purchased from Sigma–Aldrich (Milano, Italy). High Performance Liquid Chromatography (HPLC) gradient grade acetonitrile (ACN) was purchased by VWR International (Milano, Italy), H3PO4 (85% w/w) and ammonia solution (30% w/w) were purchased by Carlo Erba Reagents (Cornaredo, Milano, Italy). Aqueous OFL solutions were prepared and stored in the dark at 4 °C before use.
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