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, sensitive, accurate and low cost effective spectrophotometric method has been developed for the determination of Tetracycline and Doxycycline in pure and pharmaceutical formulations. The method is based on the reaction of methyldopa with 4-aminoantipyren (4-AAP) in presence of potassium ferriecyanide (PFC) in an alkaline medium. Two optimization methods were applied to determine the optimum conditions of oxidizing coupling reaction variables; univariate and design of experiment (DOE) method. The conditions effecting the reaction; pH, buffer Volume, reagent concentration, oxidant concentration, type of buffer, order of addition, time of reaction and stability were optimized . Under univariate and design
... Show MoreCefixime (CFX) was treated with sodium nitrite and hydrochloric acid for diazotization reaction followed by coupling with ?-Naphthol in alkaline medium to form, a yellow colored azo dye compound which exhibits maximum absorption (?max) at 412 nm where the concentration of (CFX) was determined spectrophotometrically. The optimum reaction conditions and other analytical parameters were evaluated. Beer’s law was obeyed in the concentration range of (1-20) ?g.mL-1 with a molar absorptivity of 34870.5 L.mol-1.cm-1. The limit of detection was found to be 0.1090 ?g.mL-1 and the Sandell's sensitivity value was 0.0130 ?g.cm-2. The proposed method could be successfully applied to
... Show MoreSimple, sensitive, accurate and inexpensive spectrophotometric methods have been developed for the determination of sulfamethoxazole (SMZ) in pure and dosage forms. This method is based on diazotization of primary amine group of sulfamethoxazole with sodium nitrite and hydrochloric acid followed by coupling with diphenylamine in acidic medium to obtain a stable blue colored dye and show a maximum absorption (max) at 530 nm. Different variables affecting the completion of reaction have been carefully optimized, following the classical univariate sequence and modified simplex method. Beer’s law is obeyed in the concentration range of (0.5-12.0 µg.mL-1) with molar absorptivity of 4.9617×104 L.mol-1.cm-1. The
... Show MoreIR, MIR, UV – Visible spectra have been studied for Cobalt chloride molecule (CoCl2. 6H2O) compound, In wide range spectra (40000 – 410) cm-1 specially MIR range. Assignment were achieved for the fundamental vibrational bands of (CoCl2 . 6H2O ) to symmetry stretching ?1 (?^+) Anti – symmetry stretching ?3(?^+), these bands are non-degenerate , and the bending band is ?2(?) is doubly degenerate thought they have activity in IR and Raman , which explain the weakness in symmetry of this molecule, the fundamental bands for the molecule are centered at the following wave numbers (615, 685, 795, 1115, 1340, 1375, 1616.35, 2091, 2386, 2410, 3364) cm-1 which are corresponding to wave lengths (16260, 14598, 12578, 8968, 7462, 7272, 6186,
... Show MoreA solid Phase Extraction (SPE) followed by HPLC-UV method is described for the simultaneous quantitative determination of nine priority pollutant phenols : Phenol, 2- and 4-Nitrophenol, 2,4-Dimethylphenol, 2-, 2,4-Di-, 2,4,6-Tri-, and Penta- chlorophenol, 4 Chloro-3-methylphenol. The phenols were separated using a C-18 column with UV detector at wave length of 280nm. The Flow of mobile phase was isocratic consisted of 50:50 Acetonitrile: phosphate buffer pH=7.1, column temperature 45 C°, Flow Rate 0.7 ml/min. Calibration curves were linear (R2 = 0.9961-0.9995). The RSDs (1.301-5.805)%, LOD(39.1- 412.4) µg/L, LOQ(118.5-1250.8) µg/L, the Robustness (1.55-4.89), Ruggedness (2.82-4.00), Repeatability (2.1-4.95), Recoveries%
... Show MoreThe aim of this study is to evaluate the levels of trace elements Magnesium (Mg), Zinc (Zn), Copper (Cu), and Selenium (Se) in blood sera of asthmatic patients by Atomic Absorption Spectrophotometry (AAS). The concentrations of Mg, Cu, and Zn have been determined by Flame Atomic Absorption spectrophotometry (FAAS), and Se with flameless Graphite Furnace Atomic Absorption Spectrophotometry (GFAAS). The study involves (55) asthmatic patients as study group and (28) subjects as control from both genders. Serum levels of Mg, Cu, and Se were significantly higher (p<0.001 for all) in patients when compared with healthy subjects, while Zn level was relatively significant (p<0.05). Our observations confirm the efficacy and applicability of (AAS) in
... Show MoreIn this paper, turbidimetric and reversed-phase ultra-fast liquid chromatography (UFLC) methods were described for the quantitative determination of ephedrine hydrochloride in pharmaceutical injections form. The first method is based on measuring the turbidimetric values for the formed yellowish white precipitate in suspension status in order to determine the ephedrine hydrochloride concentration. The suspended substance is formed as a result of the reaction of ephedrine hydrochloride with phosphomolybdic acid which was used as a reagent. The physical and chemical characteristics of the complex were investigated. The calibration graphs of ephedrine were established by turbidity method. While the second method (UFLC) was conducted using the
... Show MoreNew simple and sensitive spectrophotometric methods for the determination of paracetamol in aqueous medium were developed. The first method is based on coupling of paracetamol with p-amino-2-hydroxy sodium benzoate (AHB) in the presence of sodium periodate, as oxidizing agent, to form a brownish-orange compound which shows a λmax at 470 nm. The molar absorptivity (εmax) of the colored product was found to be (3371) l.mole1.cm-1 and Sandel’s index 0.0449 μg.cm-2. The method follows Beer’s law in the concentration range of 12.5-500.0 μg of paracetamol in a final volume of 25 ml (0.5-20.0) μg.ml-1 with relative standard deviation percent (R.S.D%) ranged between 0.26-4.71% and accuracy, expressed by recover
... Show MoreNew simple and sensitive spectrophotometric methods for the determination of paracetamol in aqueous medium were developed. The first method is based on coupling of paracetamol with p-amino-2-hydroxy sodium benzoate (AHB) in the presence of sodium periodate, as oxidizing agent, to form a brownish-orange compound which shows a λmax at 470 nm. The molar absorptivity (εmax) of the colored product was found to be (3371) l. mole1. cm-1 and Sandel’s index 0.0449 μg. cm-2. The method follows Beer’s law in the concentration range of 12.5-500.0 μg of paracetamol in a final volume of 25 ml (0.5-20.0) μg. ml-1 with relative standard deviation percent (RSD%) ranged between 0.26-4.71% and accuracy, expressed by recovery percent, 95-106% for five
... Show MoreA method was developed that offers a rapid, simple and accurate technique for the determination of chlorophenols at trace levels in aqueous samples with very limited volumes of organic solvents. These compounds were acetylated, then preliminarily extracted with n-hexane. The enriched chlorophenols were directly analyzed using gas chromatography with an electron-capture detector. The detection limits were in the range of 0.001–0.005 mg/L, except for 2-chlorophenol, which was always above 0.013 mg/L. Relative standard deviation for the spiked water samples ranged from 2.2 to 6.1%, while relative recoveries were in the range of 67.1 to 101.3%.