The present study combines UV-Vis spectrophotometry and dispersive liquid-liquid microextraction (DLLME) for the preconcentration and determination of trace level clidinium bromide (Clid) in pharmaceutical preparation and real samples. The method is based on ion-pair formation between Clid and bromocresol green in aqueous solution using citrate buffer (pH = 3). The colored product was first extracted using a mixture of 800 µL acetonitrile and 300 µL chloroform solvents. Then, a spectrophotometric measurement of sediment phase was performed at λ = 420 nm. The important parameters affecting the efficiency of DLLME were optimized. Under the optimum conditions, the calibration graphs of standard -1 (Std.), drug, urine and serum were ranged 0.005 - 0.16 µg mL . The limits of detection, quantification, and Sandell's sensitivity were calculated. Good recoveries of Clid Std., drug, urine and serum at 0.005, 0.01, -1 0.1 and 0.16 µg mL ranged 93.77 - 101.0%. Enrichment factor was calculated for Std., drug, urine and serum. The method was applied successfully to determine Clid in pharmaceutical preparation and real samples.
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 MoreGenistein (GEN) is one of the predominant dietary isoflavones found in legumes such as soybeans. Genistein has been recommended as an osteoporosis treatment for postmenopausal women and elderly men, with the intention of reducing cardiovascular disease and hormone-dependent malignancies. Therefore, two sensitive and simple methods for quantifying it in the supplements preparation were developed.The first method (A) comprised employing the surfactant Triton X-114 to extract the result of the diazotization reaction with 4-Aminoacetophenone(4AMA) utilizing a cloud point extraction technique. The product was extracted using micelles of a non-ionic surfactant (TritonX-114) and then spectrophotometrically detected at a specified wa
... Show MoreVerapamil Hydrochloride (VH) has been determined spectrophotometrically by using Methyl Orange (MO). In our previous researches MO was used for determination of Mexiletine Hydrochloride [1]. The method was based on complexation between (MO and VH). After shaking and diluting the complex solution with D.W, the pH was adjusted with NaOH and HCl to pH 4. The colored complex formed between VH and the reagents were transferred into separating funnels and extracted using 4.5 ml CH2Cl2 and were shaken for (4 minutes). The extracted organic layer was used for the preparation of the calibration curves for spectrophotometric measurements of VH at 437nm. The blanks were carried out in exactly the same way throughout the whol
... Show MoreA simple, fast, and sensitive batch and flow injection spectrophotometric
methods have been developed for the determination of clonazepam(CZP) in pure
form and in pharmaceutical preparations. The proposed methods are based on the
oxidative coupling reaction of the reduced clonazepam using Zn powders and conc.
HCl with payrocatechol and in the presence of ferric sulphate. The resulting reddish
colored product had a maximum absorbance at 515 nm. The optimum reaction
conditions and other analytical parameters have been evaluated . The linear ranges
for the batch and FI methods determination of CZP were 0.5-32, 50-400 μg mL-1
and the detection limits were 0.193, 22.60 μg mL-1 for both methods respectively.
Statis
A simple, accurate, and cost-efficient UV-Visible spectrophotometric method has been developed for the determination of naphazoline nitrate (NPZ) in pure and pharmaceutical formulations. The suggested method was based on the nucleophilic substitution reaction of NPZ with 1,2-naphthoquinone-4-sulfonate sodium salt in alkaline medium at 80°C to form an orange/red-colored product of maximum absorption (λmax) at 483 nm. The stoichiometry of the reaction was determined via Job's method and limiting logarithmic method, and the mechanism of the reaction was postulated. Under the optimal conditions of the reaction, Beerʼs law was obeyed within the concentration range 0.5–50 μg/mL, the molar absorptivity value (ε) was 5766.5 L × mol–1 × c
... Show MoreSimple, economic and sensitive mathematical spectrophotometric methods were developed for the estimation 4-aminoantipyrine in presence of its acidic product. The estimation of binary mixture 4-aminoantipyrine and its acidic product was achieved by first derivative and second derivative spectrophotometric methods by applying zero-crossing at (valley 255.9nm and 234.5nm) for 4-aminoantipyrine and (peak 243.3 nm and 227.3nm) for acidic product. The value of coefficient of determination for the liner graphs were not less than 0.996 and the recovery percentage were found to be in the range from 96.555 to 102.160. Normal ratio spectrophotometric method 0DD was used 50 mg/l acidic product as a divisor and then measured at 299.9 nm with correlat
... Show MoreSimple, economic and sensitive mathematical spectrophotometric methods were developed for the estimation 4-aminoantipyrine in presence of its acidic product. The estimation of binary mixture 4-aminoantipyrine and its acidic product was achieved by first derivative and second derivative spectrophotometric methods by applying zero-crossing at (valley 255.9nm and 234.5nm) for 4-aminoantipyrine and (peak 243.3 nm and 227.3nm) for acidic product. The value of coefficient of determination for the liner graphs were not less than 0.996 and the recovery percentage were found to be in the range from 96.555 to 102.160. Normal ratio spectrophotometric method 0DD was used 50 mg/l acidic product as a divisor
... 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 MoreAn accurate and sensitive spectrophotometric method has been developed for the determination of cefotaxime (CEF) in pure and pharmaceutical samples. The suggested method depended on the coupling reaction between diazotized cefotaxime and 3,5-dimethyl phenol (3,5-DMPH) in basic medium to form light orange, water soluble dye, that is stable and has a maximum absorbance at 497nm. The calibration graph was liner over the concentration range (1-70) µg.mL-1 with LOD of 0.750 µg.mL-1 and LOQ of. 2.740 µg. mL-1, sandal sensitivity of 0.0526 µg. cm-2 . molar absorptivity 11328 Lmol-1 cm-1 . The stoichiometry composition was found by Jobs a
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