This 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 values were 2.37 and7.11 µg.ml-1 respectively. The second method based on extraction of traces amounts of MET using the cloud-point extraction (CPE). This method implicated for using of a nonionic surfactant (Triton x-114) as an extraction medium which was entrap the hydrophobic complex formed between MET and nickel(ii) in basic medium as reaction system for designing the CPE procedure. The optimum conditions were similar the first method expect the amount of surfactant which was 0.5 ml. The concentrations range of calibration curve from 3.5to100 µg.ml-1 and molar absorptivity of 1.2x104 L.mol-1.cm-1. In this method was access to less of concentrations in Limit of detection and quantitation which were 0.74and 2.22 µg.ml-1 respectively. The precise (RSD %) and accuracy (recovery %) of both methods were ranged between 0.24-0.47, 97.86-98.68 respectively. The data of two methods were appeared high acceptable with standered of British Pharmacopoeia through using statistic methods (f-test and t-test), that they may be used in analysis of MET.
Cloud point extraction is a simple, safe, and environmentally friendly technique for preparing many different kinds of samples. In this review, we discussed the CPE method and how to apply it to our environmental sample data. We also spoke about the benefits, problems, and likely developments in CPE. This process received a great deal of attention during preconcentration and extraction. It was used as a disconnection and follow-up improvement system before the natural mixtures (nutrients, polybrominated biphenyl ethers, pesticides, polycyclic sweet-smelling hydrocarbons, polychlorinated compounds, and fragrant amines) and inorganic mixtures were examined and many metals like (silver, lead, cadmium, mercury, and so on). We also find
... Show MoreA 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 ma
... Show MoreA simple, rapid, sensitive and inexpensive approach is described in this work based on a combination of solid‐phase extraction of 8‐hydroxyquinoline (8HQ), for speciation and preconcentration of Cr(III) and Cr(VI) in river water, and the direct determination of these species using a flow injection system with chemiluminescence detection (FI–CL) and a 4‐diethylamino phenyl hydrazine (DEAPH)–hydrogen peroxide system. At different pH, the two forms of chromium [Cr(III) and Cr(VI)] have different exchange capacities for 8HQ, therefore two columns were constructed; the pH of column 1 was adjusted to pH 3 for retaining Cr(III) and column 2 was adjusted to pH 1 for retaining of Cr(VI). The sorbe
Ultrasonic Extraction method followed by gradient HPLC was carried out for the simultaneous determination of four insecticides are [imidacloprid (Imi), thiamethoxam (Thi), indoxacarb (Ind) and abamectin (Aba)] used to combat the major insect pests in Iraq, whitefly, Dubas Bug, worms fruits as well as to combat the spiders – dream respectively in eco-soil samples. The extraction recovery was in the range of 99.77 to 109.1 %. The dissipation kinetics and residual levels of these insecticides in soil sample was studied under field ecosystem. The half-life of the mix insecticides was determined. The half-life was in range of 0.38 to 4.06 days with the soil samples were brought from the Agricultural Land called Nahrawan located in th
... Show MoreA simple, economical and selective method employing ion pair dispersive liquid−liquid microextraction (DLLME) coupled with spectrophotometric determination of carbamazepine (CBZ) in pharmaceutical preparations and biological samples was developed. The method is based on reduction of Mo(VI) to Mo(V) using a combination of ammonium thiocyanate and ascorbic acid in acidic medium to form a red binary Mo(V) thiocyanate complex. After addition of CBZ to the complex, extraction of the formed CBZ−Mo(V)−(SCN)6 was performed using a mixture of methylene chloride and methanol. Then, the measurement of target complex was performed at the wavelength of 470 nm. The important extraction parameters affecting the efficiency of DLLME were studied and o
... Show MoreThe current work is characterized by simplicity, accuracy and high sensitivity Dispersive liquid - Liquid Micro Extraction (DLLME). The method was developed to determine Telmesartan (TEL) and Irbesartan (IRB) in the standard and pharmaceutical composition. Telmesartan and Irbesartan are separated prior to treatment with Eriochrom black T as a reagent and formation ion pair reaction dye. The analytical results of DLLME method for linearity range (0.2- 6.0) mg /L for both drugs, molar absorptivity were (1.67 × 105- 5.6 × 105) L/ mole. cm, limit of detection were (0.0242and0.0238), Limit of quantification were (0.0821and0.0711), the Distribution coefficient were
... Show MoreThe new organic reagent 2-[Benzo thiazolyl azo]-4,5-diphenyl imidazole was prepared and used as complexing agent for separation and spectrophotometric determination of Cu2+ ion in some samples include plants, soil, water and human blood serum. Initially determined all factors effect on extraction method and the results show optimum pH was (pHex=9), optimum concentration was 40?g/5mLCu2+ and optimum shaking time was (15min.), as well stoichiometry study appears the complex structure was 1:1 Cu2+: BTADPI. Interferences effect of cations were studied. Synergism effect shows MIBK gave increasing in distribution ratio (D). Organic solvent effect appears there is no any linear relation between dielectric constant for organic solvent used and dis
... Show MoreNew, simple and sensitive batch and reverse FIA spectrophotometric methods for the determination of doxycycline hyclate in pure form and in pharmaceutical preparations were proposed. These methods based on oxidative coupling reaction between doxycycline hyclate and 3-methylbenzothiazolinone-2-hydrazone hydrochloride (MBTH) in the presence ammonium ceric sulfate in acidic medium, to form green water-soluble dye that is stable and has a maximum absorbance at 626 nm. A calibration graph shows that a Beer's law is obeyed over the concentration range of 1-80 and 0.5-110 ?g.mL-1 of DCH for the batch and rFIA respectively with detection limit of 0.325 ?g.mL-1 of DCH for r-FIA methods. All different chemicals and physical experimental paramete
... Show MoreA batch and flow injection (FI) spectrophotometric methods are described for the determination of barbituric acid in aqueous and urine samples. The method is based on the oxidative coupling reaction of barbituric acid with 4-aminoantipyrine and potassium iodate to form purple water soluble stable product at λ 510 nm. Good linearity for both methods was obtained ranging from 2 to 60 μg mL−1, 5–100 μg mL−1 for batch and FI techniques, respectively. The limit of detection (signal/noise = 3) of 0.45 μg mL−1 for batch method and 0.48 μg mL−1 for FI analysis was obtained. The proposed methods were applied successfully for the determination of barbituric acid in tap water, river water, and urine samples with good recoveries of 99.92
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