A new attempt is made to determine diosmin (DIO) in its pure form and in dietary supplements by using spectrophotometric flow injection analysis (FIA) assay method conjugated with batch method. The analysis was achieved depending on the oxidative coupling reaction with N, N-dimethyl-p-phenylenediamine (DMPD) to form a green dye which is measured at wavelength of 677 nm. The tested methods were found to be economical, delicate, precise and sturdy. The validation variables of the batch and FIA methods gave linearity in the determination range of DIO (1-35) μg/mL and (5-120) μg/mL demonstrated calibration graphs with linearity coefficient values of r2 =0.9989 and r2 =0.9991, respectively. Limits of quantitation (LOQ) values were found to be (0.8463 and 1.022) μg/mL, while limits of detection (LOD) were (0.2539 and 0.3067) µg/mL for the two methods, respectively. The precision for the developed methods denoted by relative standard deviation (RSD %), were 0.386 and 0.55 %, while the accuracy based on recovery values (Rec %) were 100.273 and 100.24, respectively. The relative error (RE %) was less than 1% for the batch method and (1.1%) for the FIA method. The values of these parameters were observed to fall within the specified accepted limits; therefore, the tested methods seem to be adequate for the analysis of DIO in pharmaceutical preparations.
New, simple and accurate batch and flow injection spectrophotometric
methods have been developed for the determinationsof tetracycline
hydrochloride (TCH) and doxycycline hyclate (DCH) in pharmaceutical
preparations. The methods are based on diazotization of
metchlopramide and coupling reaction with either TCH or DCH in alkaline
medium to form yellow–orange water soluble dye with absorption maxima
at 414 and 436 nm for TCH and DCH, respectively. A graphs of absorbance
versus concentration show that Beer’s law was obeyed over the
concentration ranges of 1 –52 μgmL-1 TCH and DCH for batch method and
of 8 – 240 μg mL-1 TCH and 5 – 350 μgmL-1 DCH for FIA method. The
limits of detection in batchmetho
Simple and sensitive spectrophotometric method is described based on the coupling reaction of tetracycline hydrochloride (TC. HCl) with diazotized 4-aminopyridine in bulk and pharmaceutical forms. Colored azo dye formed during this reaction is measured at 433 nm as a function of time. Factors affecting the reaction yield were studied and the conditions were optimized. The kinetic study involves initial rate and fixed time (10 minutes) procedures for constructing the calibration graphs to determine the concentration of (TC. HCl). The graphs were linear for both methods in concentration range of 10.0 to 100.0 μg.mL-1. The recommended procedure was applied successfully in the determination of (TC. HCl) in its commercial formulations.
Simple and sensitive kinetic methods are developed for the determination of Paracetamol in pure form and in pharmaceutical preparations. The methods are based on direct reaction (oxidative-coupling reaction) of Paracetamol with o-cresol in the presence of sodium periodate in alkaline medium, to form an intense blue-water-soluble dye that is stable at room temperature, and was followed spectrophotometriclly at λmax= 612 nm. The reaction was studied kinetically by Initial rate and fixed time (at 25 minutes) methods, and the optimization of conditions were fixed. The calibration graphs for drug determination were linear in the concentration ranges (1-7 μg.ml-1) for the initial rate and (1-10 μg.ml-1) for the fixed time methods at 25 min.
... Show MoreNew, simple and sensitive batch and Flow-injecton spectrophotometric methods for the determination of Thymol in pure form and in mouth wash preparations have been proposed in this study. These methods were based on a diazotization and coupling reaction between Thymol and diazotized procaine HCl in alkaline medium to form an intense orange-red water-soluble dye that is stable and has a maximum absorption at 474 nm. A graphs of absorbance versus concentration show that Beer’s law is obeyed over the concentration range of 0.4-4.8 and 4-80 µg.ml-1 of Thymol, with detection limits of 0.072 and 1.807 µg.ml-1 of Thymol for batch and FIA methods respectively. The FIA procedure sample throughput was 80 h-1. All different chemical and physical e
... Show MoreA simple analytical method was used in the present work for the simultaneous quantification of Ciprofloxacin and Isoniazid in pharmaceutical preparations. UV-Visible spectrophotometry has been applied to quantify these compounds in pure and mixture solutions using the first-order derivative method. The method depends on the first derivative spectrophotometry using zero-cross, peak to baseline, peak to peak and peak area measurements. Good linearity was shown in the concentration range of 2 to 24 μg∙mL-1 for Ciprofloxacin and 2 to 22 μg∙mL-1 for Isoniazid in the mixture, and the correlation coefficients were 0.9990 and 0.9989 respectively using peak area mode. The limits of detection (LOD) and limits of quantification (LOQ) wer
... Show MoreDevelopment of a precise and delicate reaction has been acquired for the determination of vancomycin hydrochloride using batch and cloud point extraction (CPE) methods. The first method is based on the formation of azo dye as a result of diazotized dapsone coupled with vancomycin HCl (VAN) in a basic medium. The sensitivity of this reaction was enhanced by utilizing a nonionic surfactant (Triton X-114) and the cloud point extraction technique (second method). The azo dye formed was extracted into the surfactant-rich phase, dissolved in ethanol and detected at λmax 440 nm spectrophotometrically. The reaction was investigated using both batch and CPE methods (with and without extraction), and a simple comparison between the two
... Show MoreA new method for determination of allopurinol in microgram level depending on its ability to reduce the yellow absorption spectrum of (I-3) at maximum wavelength ( ?max 350nm) . The optimum conditions such as "concentration of reactant materials , time of sitting and order of addition were studied to get a high sensitivity ( ? = 27229 l.mole-1.cm-1) sandal sensitivity : 0.0053 µg cm-2 ,with wide range of calibration curve ( 1 – 9 µg.ml-1 ) good stability (more then24 hr.) and repeatability ( RSD % : 2.1 -2.6 % ) , the Recovery % : ( 98.17 – 100.5 % ) , the Erel % ( 0.50 -1.83 % ) and the interference's of Xanthine , Cystein , Creatinine , Urea and the Glucose in 20 , 40 , 60 fold of analyate were also studied .
A reliable differential pulse polarographic (DPP) method has been developed and applied for the determination of ibuprofen IBU in dosage form with dropping mercury electrode (DME) versus Ag/AgCl. The best peak was found at cathodic peak of -1.18 V in phosphate buffer at pH=4 and 0.025M of KNO3 as supporting electrolyte. In order to obtaine the highest sensitivity, instrumental and experimental parameters were examined including the type and concentration of supporting electrolyte, pH of buffer solution, pulse amplitude and voltage step time. Diffusion current showed a direct linear relationship to ibuprofen concentration in the range of (5 – 30) μg. mL-1 (2.43× 10-5
... Show MoreDetermining the actual amounts of active ingredients in various pharmaceutical commercial forms is still receiving a lot of attention. Two flow injection analysis (FIA) methods were suggested for determination of mesalazine (MES) in pharmaceutical forms. Normal and reverse FIA systems (nFIA and rFIA) combined with UV-Vis spectrophotometric technique were used for the analysis. The methods involved using two mods of FIA systems for measuring a colored product result from coupling of MES with 2,2'-dihydroxybiphenyl after oxidized with sodium periodate in alkaline medium. The absorbance of the red colored dye was measured at maximum wavelength of 500 nm. The calibration graphs for MES were linear in the ranges 2.5-200 and 0.5-60 µg/mL with
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