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 parameters affecting the development and stability of the colored product were carefully studied. The proposed methods were successfully applied for the determination of DCH in pharmaceutical preparations.
This research presents a new study in reactive distillation by using consecutive reaction: the saponification reaction of diethyl adipate (DA) with sodium hydroxide solution .
The effect of three parameters were studied through a design of experiments applying 23 factorial design . These parameters were : the mole ratio of DA to NaOH solution (0.1 and 1) , NaOH solution concentration (3 N and 8 N) , and batch time (1.5 hr. and 3.5 hr.) . The conversion of DA to sodium monoethyladipate(SMA)(intermediate product) was the effect of these parameters which was detected . Also , the percentage purity of the intermediate product was recorded . The results showed that increasing mole ratio of DA to NaOHsolutio
... Show MoreA new mode of methodology was adopted in the assay of PM- HCL based on the use of water crystal gel bead made of poly acrylic acid in which the gel beads were left to absorbe persulphate solution that is necessary for the oxidation of PM- HCL in aqua media . The water crystal act as a reserviour for S2O82- . Optimum parameters were studied giving to specify the chemical and physical parameters. Two line manifold was used .The flow rates of 1.5 and 1.2 ml.min-1 was used , 3 gel beads , 120 μL sample volume , a linear dynamic range extend from 0.01- 18 mmol.L-1. A correlation coefficient (r) of 0.9991while the percentage linearity (r2%) of 99.82% with R.S.D% at 8 mmol.L-1 promethazine-HCl is less than 0.5% (ten replicates) and a detection
... 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 MoreA newly developed analytical method characterized by its speed and sensitivity for the determination of metformin-HCl via the formation of complex for metformin-HCl-OH--copper(II) ion from the gel bead system by continuous flow injection analysis. The method is based on the imbedded copper(II) ion in the gel bead structure can be used in the reaction for the formation of red –magneta colour complex(λmax. =530nm) formed by direct reaction of the drug with the released copper (II) ion from the gel bead in alkaline medium. Linear dynamic range for the absorbance versus metformin concentration was 0.001-1 mmol.L-1 while C.O.D was (r2% =95.33%) . The L.O.Q was 0.868mmol.L-1.L.O.D (S/N=3)=0.5μmol.L-1 from the step wise dilution for the min
... Show MoreA new, Simple, sensitive and accurate spectrophotometric methods have been developed for the determination of sulfanilamide (SNA) drug in pure and in synthetic sample. This method based on the reaction of sulfanilamide (SNA) with 1,2-napthoquinone-4-sulphonic acid (NQS) to form N-alkylamono naphthoquinone by replacement of the sulphonate group of the naphthoquinone sulphonic acid by an amino group. The colored chromogen shows absorption maximum at 455 nm. The optimum conditions of condensation reaction forms were investigated by: (1) univariable method, by optimizing the effect of experimental variables; (different bases, reagent concentration, borax concentration and reaction time), (2) central composite design (CCD) including
... 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.
Simple and rapid spectrophotometric determination of furosemide (FUR) has been investigated .The method is based on acid hydrolysis of FUR to free primary aromatic amine and diazotization followed by coupling with 3, 5 di methyl phenol (3, 5-DMPH) at basic medium. The absorbance was measured at 434 nm, the method was optimized for best condition, and beers’ law is obeyed over the range of 0.4-50 µg.mL-1 with molar absorptivity and sandal’s sensitivity 1.3899 x104 L moL-1 .cm-1 and 0.0238x104 µg.cm-2 respectively. Analysis of solution containing nineteen different concentrations of FUR gave a correlation coefficient of (0.9999) a
... Show MoreA series of lanthanide metal (???) complexes have been prepared from the new azo ligand, 3-(1-methyl-2-benzimidazolylazo)-Tyrosine (MBT). The structural feature were confirmed on the basis of their elemental analysis, metal content, molar conductance, magnetic measurement, FTIR, 1 HNMR and UV-Vis spectra studies. The isolated complexes were found to have a mole ratio (1:2) (metal:ligand) stoichiometry with the general formula [Ln(MBT)2]Cl (Ln(???) = La, Ce, Pr, Nd, Sm, Eu and Gd). The chelates were found to have octahedral structures. The FTIR spectra shows that the ligand (MBT) is coordinated to lanthanide ions as a N, N, O-tridentate anion via benzimidazole nitrogen, azo nitrogen and oxygen of hydroxyl after deprotonation. Com
... Show MoreA simple, sensitive and rapid method was used for the estimate of: Propranolol with Bi (III) to prove the efficiency, reliability and repeatability of the long distance chasing photometer (NAG-ADF-300-2) using continuous flow injection analysis. The method is based on a reaction between propranolol and Bi (III) in an aqueous medium to obtain a yellow precipitate. Optimum parameters were studied to increase the sensitivity for the developed method. A linear range for calibration graph was 0.1-25 mmol/L for cell A and 1-40 mmol/L for cell B, and LOD 51.8698 ng/200 µL and 363.0886 ng /200 µL , respectively to cell A and cell B with correlation coefficient (r) 0.9975 for cell A, 0.9966 for cell B, RSD% was lower than 1%, (n = 8) for the
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