A simple and novel method was developed by combination of dispersive liquid-liquid microextraction with UV spectrophotometry for the preconcentartion and determination of trace amount of malathion. The presented method is based on using a small volume of ethylenechloride as the extraction solvent was dissolved in ethanol as the dispersive solvent, then the binary solution was rapidly injected by a syringe into the water sample containing malathion. The important parameters, such the type and volume of extraction solvent and disperser solvent, the effect of extraction time and rate, the effect of salt addition and reaction conditions were studied. At the optimum conditions, the calibration graph was linear in the range of 2-100 ng mL-1 of malathion with a limit of detection of 0.8 ng L-1. In addition, the enrichment factor was 30. The developed method was successfully applied for the determination of malathion pesticide in water samples.
A simple, precise, rapid, and accurate reversed – phase high performance liquid chromatographic method has been developed for the determination of guaifenesin in pure from pharmaceutical formulations.andindustrial effluent. Chromatography was carried out on supelco L7 reversed- phase column (25cm × 4.6mm), 5 microns, using a mixture of methanol –acetonitrile-water: (80: 10 :10 v/v/v) as a mobile phase at a flow rate of 1.0 ml.min-1. Detection was performed at 254nm at ambient temperature. The retention time for guaifenesin was found 2.4 minutes. The calibration curve was linear (r= 0.9998) over a concentration range from 0.08 to 0.8mg/ml. Limit of detection (LOD) and limit of quantification ( LOQ) were found 6µg/ml and 18µg/ml res
... Show MoreAbstract :In this study, amygdaline in Iraqi plant seeds was extracted and isolated from their seeds matrix using reflux procedure and subsequently identified and determined by high performance liquid chromatography (HPLC) on reversed phase column of LC-18 (150mm x 4.6mm, 5?m )with actonitrile :water ( 50 : 50 ) as mobile phase at flow rate of ( 0.5 mL/min ) and detection at wavelength of 215 nm.The experimental results indicated that the linearity of calibration is in the range of 1.0-30.0 mg L-1amygdaline with the correlation coefficient of 0.9949. The limit of detection (LOD) and limit of quantitation (LOQ) for amygdaline were of 0.88 and 2.93 mg L-1 in standard pure sample. The mean recovery percent is 97.34±0.58 at 95% confidence inte
... Show MoreThis work was influenced the separation and preconcentration steps were carried out to determination of metformin (MET) in pharmaceutical preparations and human serum samples. Complex formation method and cloud-point extraction (CPE) coupling with UV-Visible spectrophotometry were used to investigated of study target.The results has showed the best optical characteristic for calibration curve and statistical data which were obtained under optimum conditions. The first method is based on the reaction of MET with nickel (II) in alkaline medium an absorption maximum ?)max) at 434nm. ''Beer's low'' is obeyed in the concentration range (10-100µg.ml-1) with molar absorptivity of 3.9x103 L.mol-1.cm-1.The limit of detection and quantitation valu
... Show MoreThe development of a reversed phase high performance liquid chromatography fluorescence method for the determination of the mycotoxins fumonisin B1 and fumonisin B2 by using silica-based monolithic column is described. The samples were first extracted using acetonitrile:water (50:50, v/v) and purified by using a C18 solid phase extraction-based clean-up column. Then, pre-column derivatization for the analyte using ortho-phthaldialdehyde in the presence of 2-mercaptoethanol was carried out. The developed method involved optimization of mobile phase composition using methanol and phosphate buffer, injection volume, temperature and flow rate. The liquid chromatographic separation was performed using a reversed phase Chromolith® RP-18e column
... Show MoreA simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected opti
... Show MoreA simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected optimum conditions,
... Show MoreLiquid electrodes of domperidone maleate (DOMP) imprinted polymer were synthesis based on precipitation polymerization mechanism. The molecularly imprinted (MIP) and non-imprinted (NIP) polymers were synthesized using DOMP as a template. By methyl methacrylate (MMA) as monomer, N,Nmethylenebisacrylamide (NMAA) and ethylene glycol dimethacrylate (EGDMA) as cross-linkers and benzoyl peroxide (BP) as an initiator. The molecularly imprinted membranes were synthesis using acetophenone (APH), di-butyl sabacate (DBS), Di octylphthalate (DOPH) and triolyl phosphate (TP)as plasticizers in PVC matrix. The slopes and limit of detection of l
... Show MoreThis research investigates manganese (Mn) extraction from Electric Arc Furnace Steel Slag (EAFS) by using the Liquid-liquid extraction (LLE) method. The chemical analysis was done on the slag using X-ray fluorescence, X-ray diffraction, and atomic absorption spectroscopy. This work consisted of two parts: the first was an extensive study of the effect of variables that can affect the leaching process rate for Mn element from slag (reaction time, nitric acid concentration, solid to liquid ratio, and stirring speed), and the second part evaluates the extraction of Mn element from leached solution. The results showed the possibility of leaching 83.5 % of Mn element from the slag at a temperature of 25°C, nitric acid co
... Show MoreA single step extraction-cleanup procedure using porous membrane-protected micro-solid phase extraction (μ-SPE) in conjunction with liquid chromatography–tandem mass spectrometry for the extraction and determination of aflatoxins (AFs) B1, B2, G1 and G2 from food was successfully developed. After the extraction, AFs were desorbed from the μ-SPE device by ultrasonication using acetonitrile. The optimum extraction conditions were: sorbent material, C8; sorbent mass, 20 mg; extraction time, 90 min; stirring speed, 1000 rpm; sample volume, 10 mL; desorption solvent, acetonitrile; solvent volume, 350 μL and ultrasonication period, 25 min without salt addition. Under the optimum conditions, enrichment factor of 11, 9, 9 and 10 for AFG2, AFG1
... Show MoreEmulsion Liquid Membrane (ELM) is an emerging technology that removes contaminants from water and industrial wastewater. This study investigated the stability and extraction efficiency of ELM for the removal of Chlorpyrifos Pesticide (CP) from wastewater. The stability was studied in terms of emulsion breakage. The proposed ELM included n-hexane as a diluent, span-80 as a surfactant, and hydrochloric acid (HCl) as a stripping agent. Parameters such as mixing speed, aqueous feed solution pH, internal-to-organic membrane volume ratio, and external-to-emulsion volume ratio were investigated. A minimum emulsion breakage of 0.66% coupled with a maximum chlorpyrifos extraction and stripping efficiency were achieved at 96.1% and 95.7% at b
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