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.
The simple and available technique of colorimetry and indirect X-ray fluorescence determination of tetracycline hydrochloride (in the form of colored complex with iron(III) ions) and cyanocobalamine (in the form of the colored thiocyanate complex with cobalt(II) ions) is offered. The analytes were separated from the accompanying components by sorption to polyurethane foam based on ethers. The conditions of sorption separation and measurement of analytical signal of these substances are optimized. The obtained results of tetracycline drugs and injection solution B12 vitamin are in satisfactory agreement with data declared by the manufacturer.
A simple, low cost and rapid flow injection turbidimetric method was developed and validated for mebeverine hydrochloride (MBH) determination in pharmaceutical preparations. The developed method is based on forming of a white, turbid ion-pair product as a result of a reaction between the MBH and sodium persulfate in a closed flow injection system where the sodium persulfate is used as precipitation reagent. The turbidity of the formed complex was measured at the detection angle of 180° (attenuated detection) using NAG dual&Solo (0-180°) detector which contained dual detections zones (i.e., measuring cells 1 & 2). The increase in the turbidity of the complex was directly proportional to the increase of the MBH concentration
... Show MoreA simple, low cost and rapid flow injection turbidimetric method was developed and validated for mebeverine hydrochloride (MBH) determination in pharmaceutical preparations. The developed method is based on forming of a white, turbid ion-pair product as a result of a reaction between the MBH and sodium persulfate in a closed flow injection system where the sodium persulfate is used as precipitation reagent. The turbidity of the formed complex was measured at the detection angle of 180° (attenuated detection) using NAG dual&Solo (0-180°) detector which contained dual detections zones (i.e., measuring cells 1 & 2). The increase in the turbidity of the complex was directly proportional to the increase of the MBH concentration
... Show MoreNew metal complexes of the ligand 4-[5-(2-hydoxy-phenyl)-[1,3,4- oxadiazol -2-ylimino methyl]-1,5-dimethyl-2-phenyl-1,2-dihydro-pyrazol-3-one (L) with the metal ions Co(II), Ni(II), Cu(II) and Zn(II) were prepared in alcoholic medium. The Schiff base was synthesized through condensate of [4-antipyrincarboxaldehyde] with[2-amino-5-(2-hydroxy-phenyl-1,3,4- oxadiazol] in alcoholic medium . Two tetradentate Schiff base ligand were used for complexation upon two metal ions of Co2+, Ni2+, Cu2+ and Zn2+ as dineucler formula M2L2.4H2O. The metal complexes were characterized by FTIR Spectroscopy, electronic Spectroscopy, elemental analysis, magnetic susceptidbility measurements, and also the ligand was characterized by 1H-NMR spectra, and m
... Show More2(2-Tetrahydropyranylthio) methyl cyclopropyl amines were synthesized from allylmercaptan through several steps. The structures of the intermediates and the final products where confirmed through IR, NMR and elemental analysis, these compounds may be of value in the treatment of diseases where free radicals are implicated in their pathogensis, since the thio and the amino groups of the synthesized compounds may act as free radical scavengers.
A cost-effective and efficient detector was created to conduct thorough turbidimetric measurements by reaction of Co (II) ion with calcium ferro cyanide to form bright green particulate, using the method of continuous flow injection analysis, the use of NAG-5SX1-1D-SSP Analyzer in determining cobalt (II) ion in a test for the validity of the new design. The NAG-5SX1-1D-SSP Analyzer is composed of five irradiation sources of white snow leds having the diameter of 10 mm with one solar cell of 55 mm length, 13.5 mm width. Using a selector switch to select the optimum voltage to be used which was 2.7 VDC. Under conditions of optimization, cobalt (II) ion was determined at 0.005–20 mmol. L–1(n = 23) while linearity dynamic range 0.005–7 mm
... Show MoreA simple, sensitive and accurate spectrophotometric method has been developed for the determination of salbutamol sulphate (SAB) and isoxsuprine hydrochloride (ISX) in pure and pharmaceutical dosage. The method involved oxidation of (SAB) and (ISX) with a known excess of N-bromosuccinamid in acidic medium, and subsequent occupation of unreacted oxidant in decolorization of Evans blue dye (EB). This, in the presence of SAB or ISX was rectilinear over the ranges 1.0-12.0, 1.0-11.0 µg/mL, with molar absorptivity 4.21×104 and 2.58×104 l.mol-1.cm-1 respectively. The developed method had been successfully applied for the determination of the studied drugs in their pharmaceutical dosage resulting i
... Show More2- amino -5- thiol-1,3,4- thiadiazole (S1) was prepared by cyclic locking of thiosemicarbazide in the presence of anhydrous sodium carbonate and CS2. diazotization of (S1) compound gave diazonium salt (S2) that reacts with different activated aromatic compounds to get the following azo compounds ,2 [(4- aminophenyl) diazenyl ] 1,3,4- thiazdiazole-5- thiol (S3) ,2-[4-amino- 1-naphthyl diazenyl] -1,3,4 – thiazdiazole-5-thiol (S4) , 3-amino-4-[(5- mercapto -1,3,4- thiadiazole -2-yl) diazenyl ] phenol(S5) ,1-[(5-mercapto-1,3,4-thiadiazole-2-yl) diazenyl] -2-naphthol (S6) , 5-{[4-(dimethylamino) phenyl] diazenyl}-1,3,4-thiadiazole-2- thiol(S7) ,5-{[4-(diethylamino) phenyl] diazenyl}-1,3,4- thiadiazole-2- thiol(S8) ,2- amino-5-[(5-mercapto-1,3
... Show MoreIsocratic high performance liquid chromatography on reversed phase a (150x 4.6 mm I.D), 5 ?m ?-Bondapak RP-8 column (with acidic mobile phase allow the separation of doxcycycline hydrochloride with low detection limit of 0.2 µg/ml detected by UV set at 226 nm. The method was validated for Doxycycline between 0.156- to 5 µg/ml. The concentration of doxycycline was assessed in two single dose randomized crossover studies with intervals of one week between two period. In sera of 20 adults healthy male volunteers with average age of (42 + 10) year, body weight 48-85 kg, body height of (160-185cm) after a single dose of doxycycline hydrochoride 100 mg in form of capsules were orally administrated for both formulations. The blood sa
... Show MoreA simple, precise, and sensitive spectrophotometric method has been established for the analysis of doxycycline. The method includes direct charge transfer complexation of doxycycline withp-Bromanil in acetonitrileto form a colored complex. The intensely colored product formed was quantified based on the absorption band at 377 nm under optimum condition. Beer’s law is obeyed in the concentration range of 1–50 μg.mL-1 with molar absorptivity of 1.5725x104 L.mol-1.cm-1, Sandell's sensitivity index (0.0283) μg.cm-2, detection limit of 0.1064 μg.mL-1, quantification limit 0.3224 μg.mL-1 and association constant of the formed complex (0.75x103). The developed method could find application in routine quality control of doxycycline and has
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