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.
A 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 di-(2-ethylhexyl) phthalate (DEHP) was extracted using different solvents from plastic blood bag. The extracted product was identified using FT-IR, NMR (1H and 13C), DEPT, COSY, HMBC and HSQC_TOCSY spectrometry. The extracted plasticizer was tested in complex formation with Fe2+ and Cr3+ using UV-visible spectrophotometric method. The migration of the plasticizer from the blood bags to the blood was studied and determined during different storage times depending upon the formation of complexes with Fe2+ and Cr3+, and the change in the concentration of Fe2+ and Cr3+.
The 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 MoreThis paper concerned with development of a spectrophotometric method for the determination of paracetamol, based on the diazotisation and coupling reaction with anthranilic acid in basic medium, to form an intense yellow coloured, water-soluble and stable azo-dye which shows a maximum absorption at 421nm. Beer’s law is obeyed over the concentration range of 1.0-10 µg/ml; with molar absorptivity of 2.1772×104 L.mol -1.cm-1 and Sandell’s sensitivity index 6.9446 µg.cm-2. The method has been applied successfully for the determination of paracetamol in pharmaceutical formulation.
New, 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 simple, precise and accurate spectrophotometric method has been developed for simultaneous estimation of sulfanilamide and furosemide in their mixture by using first and second order derivative method in the ultraviolet region. The method depends on first and second derivative spectrophotometry, with zero-crossing and peak to base line and peak area measurements. The first derivative amplitudes at 214, 238 and 266 nm were selected for the assay of sulfanilamide and 240, 260, 284, 314 and 352 nm for furosemide. Peak area at 201222, 222-251 and 251-281 nm selected for estimation of sulfanilamide and at 229-249, 249270, 270-294, 294-333 and 333-382 nm for furosemide. The second derivative amplitudes at 220, 252 and 274 nm for sulfanilamid
... Show MoreA simple, rapid and sensitive spectrophotometirc method for the determination of trace amounts of promethazine hydrochloride in the aqueous solution is described. The method is based on the complexation of promethazine hydrochloride with In (III) in the presence of sodium hydroxide to form an soluble product with maximum absorption at 304nm. Beer’s law is obeyed over the concentration range of (2- 20μg/ml) with molar absorptivity of (1.92× 103 L.mol-1 .cm -1 ). The optimum conditions for all development are described and the proposed method has been successfully applied for the determination of promethazine hydrochloride in bulk drug.
Samples of gasoline engine oil (SAE 5W20) that had been exposed to various oxidation times were inspected with a UV-Visible (UV-Vis) spectrophotometer to select the best wavelengths and wavelength ranges for distinguishing oxidation times. Engine oil samples were subjected to different thermal oxidation periods of 0, 24, 48, 72, 96, 120, and 144 hours, resulting in a range of total base number (TBN) levels. Each wavelength (190.5 – 849.5 nm) and selected wavelength ranges were evaluated to determine the wavelength or wavelength ranges that could best distinguish among all oxidation times. The best wavelengths and wavelength ranges were analyzed with linear regression to determine the best wavelength or range to predict oxidation t
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