scholarly journals Fingerprint Spectrophotometric Methods for the Determination of Co-Formulated Otic Solution of Ciprofloxacin and Fluocinolone Acetonide in Their Challengeable Ratio

2019 ◽  
Vol 2019 ◽  
pp. 1-14
Author(s):  
Reem H. Obaydo ◽  
Amir Alhaj Sakur
Keyword(s):  
Single Dose ◽  
Original Method ◽  
Fluocinolone Acetonide ◽  
The Other ◽  
Resolution Method ◽  
Spectrophotometric Methods ◽  
Enrichment Technique ◽  
Sample Enrichment ◽  
Constant Multiplication

Six spectrophotometric methods were developed to determine a new single-dose otic solution known as “Otovel®,” which consists of two components: the major one is ciprofloxacin (CIP) and the minor is fluocinolone acetonide (FLU). The ratio of (CIP) and (FLU) in Otovel® is 12 : 1, which is considered a challengeable ratio for UV determination. Thus, spectrum addition as a sample enrichment technique was required for the analysis of (FLU) low concentration. All these methods were capable of resolving the spectra for each component in D0 belonging to the fingerprint resolution technique. The former absorptivity centering (a-centering) method was recently developed in 2018; it was effectively applied for its solution of both binary components in Otovel®, while another method, ratio subtraction (RS), is considered as an original resolution method that could be applied to determine only one component in mixtures. However, the other four methods that are related to their original method (RS) were extended ratio subtraction (EXRS), constant multiplication (CM), unified constant subtraction (UCS), and spectrum subtraction (SS). They were also easily applied for completing the quantification of binary mixture drugs present in Otovel®. The linearity ranges were found to be 3.0–15.0 μg/mL for (CIP) and (FLU), respectively. All results acquired from the proposed methods were successfully estimated according to ICH criteria and were statistically compared with official ones where no differences were noticed.

Development and Validation of Spectrophotometric Methods for the Determination of Canagliflozin or Gliclazide and Metformin in the Presence of Metformin Impurity (1-Cyanoguanidine)

2019 ◽  
Vol 102 (4) ◽  
pp. 1112-1124
Author(s):  
Sonia T Hassib ◽  
Elham A Taha ◽  
Ehab F Elkady ◽  
Ghada H Barakat
Keyword(s):  
Second Step ◽  
Chemometric Methods ◽  
Chemometric Method ◽  
Spectrophotometric Methods ◽  
Enrichment Technique ◽  
Validation Parameters ◽  
Sample Enrichment ◽  
Development And Validation ◽  
Separation Results

Abstract Background: Quantitative multicomponent analysis is considered an analytical goal to save time and cost in analysis. Objective: This work aimed to provide sensitive and selective [successive ratio subtraction coupled with constant multiplication (SRS-CM) and chemometric] methods for the determination of coformulated antidiabetic drugs, namely canagliflozine and metformin or gliclazide and metformin in presence of metformin degradation product, 1-cyanoguanidine. Methods: SRS-CM method was developed for the determination of canagliflozin and metformin at 292 and 237 nm, respectively, using 14 μg/mL canagliflozin as a divisor in the first step to cancel the spectrum of canagliflozin. Then, 18 μg/mL metformin was used as a divisor in the second step to cancel the spectrum of metformin. Finally, we obtained the spectrum of cyanoguanidine. Chemometric method was applied for the determination of the gliclazide and metformin mixture in a 225–235 nm range. Sample enrichment technique was used to increase the concentration of canagliflozin or gliclazide to allow its simultaneous determination with metformin without prior separation. Results: Validation parameters according to the International Conference on Harmonization guidelines were satisfactory over the concentration ranges of 5 to 16 μg/mL for canagliflozin and metformin as well as 2.5 to 12.5 and 6 to 24 μg/mL for gliclazide and metformin, respectively. Conclusions: The method provides sufficient selectivity and accuracy to be applied for routine analysis and quality control in laboratories for the cited drugs. Highlights: This work shows two examples to how to select a suitable UV spectrophotometric method to overcome the spectral overlap.

The possibilities of polarography in the chemistry of nitroazoles

1984 ◽  
Vol 49 (6) ◽  
pp. 1342-1353 ◽  
Author(s):  
Dragica Dumanović ◽  
Janka Ćirić ◽  
Djuro Kosanović ◽  
Dragoslav Jeremić
Keyword(s):  
Nitro Group ◽  
Systematic Investigation ◽  
Nitro Compounds ◽  
The Other ◽  
Polarographic Method ◽  
Spectrophotometric Methods ◽  
Group Position ◽  
High Yields

Based on systematic investigation of mononitroimidazoles, selective polarographic and spectrophotometric methods for determination of nitrazole compounds in reaction mixture are proposed. It was proved that the selectivity is based on the different properties of the nitro group due to the effects of the nitro group position in the ring, the type and position of the other substituents and on the fact whether the compound is N-substituted or not. The proposed methods can be successfully used for monitoring the synthetic procedures and decreasing the number of experiments for optimization. Based on the anticipated and proved behaviour of the nitro compounds of pyrazole, novel mononitropyrazole derivatives were synthetized in a new way and with high yields. Applying the polarographic method it was discovered that during N-substitution of tautomeric mononitroimidazole and mononitropyrazole substrates other byproducts were obtained besides the main products and undesired isomers. The products were identified and then a correct and more complete N-substitution scheme could be given. Following quantitatively these N-substitution processes conclusions which directly concern the mechanism of reactions were drawn.

scholarly journals Application of Inorganic Oxidants to the Spectrophotometric Determination of Ribavirin in Bulk and Capsules

2006 ◽  
Vol 89 (2) ◽  
pp. 341-351 ◽  
Author(s):  
Ibrahim A Darwish ◽  
Alaa S Khedr ◽  
Hassan F Askal ◽  
Ramadan M Mohamed
Keyword(s):  
Ammonium Sulfate ◽  
Acid Medium ◽  
Chromium Trioxide ◽  
Potassium Dichromate ◽  
Ammonium Molybdate ◽  
The Other ◽  
Potassium Iodate ◽  
Potassium Periodate ◽  
Spectrophotometric Methods

Abstract Eight spectrophotometric methods for determination of ribavirin have been developed and validated. These methods were based on the oxidation of the drug by different inorganic oxidants: ceric ammonium sulfate, potassium permanganate, ammonium molybdate, ammonium metavanidate, chromium trioxide, potassium dichromate, potassium iodate, and potassium periodate. The oxidation reactions were performed in perchloric acid medium for ceric ammonium sulfate and in sulfuric acid medium for the other reagents. With ceric ammonium sulfate and potassium permanganate, the concentration of ribavirin in its samples was determined by measuring the decrease in the absorption intensity of the colored reagents at 315 and 525 nm, respectively. With the other reagents, the concentration of ribavirin was determined by measuring the intensity of the developed colored reaction products at the wavelengths of maximum absorbance: 675, 780, 595, 595, 475, and 475 nm for reactions with ammonium molybdate, ammonium metavanidate, chromium trioxide, potassium dichromate, potassium iodate, and potassium periodate, respectively. Different variables affecting the reaction conditions were carefully studied and optimized. Under the optimum conditions, linear relationships with good correlation coefficients (0.99840.9998) were found between the absorbance readings and the concentrations of ribavirin in the range of 41400 g/mL. The molar absorptivities were correlated with the oxidation potential of the oxidants used. The precision of the methods were satisfactory; the values of relative standard deviation did not exceed 1.64%. The proposed methods were successfully applied to the analysis of ribavirin in pure drug material and capsules with good accuracy and precision; the recovery values were 99.2101.2 0.481.30%. The results obtained using the proposed spectrophotometric methods were comparable with those obtained with the official method stated in the United States Pharmacopeia.

Determination of the lattice translation across {110} APBs in GaAs

1988 ◽  
Vol 46 ◽  
pp. 600-601
Author(s):  
D.R. Rasmussen ◽  
N.-H. Cho ◽  
C.B. Carter
Keyword(s):  
Grain Boundaries ◽  
Lower Energy ◽  
Antiphase Boundary ◽  
The Other ◽  
Boundary Structure ◽  
Interface Plane ◽  
Inversion Symmetry ◽  
High Angle ◽  
Equilibrium Distance

Domains in GaAs can exist which are related to one another by the inversion symmetry, i.e., the sites of gallium and arsenic in one domain are interchanged in the other domain. The boundary between these two different domains is known as an antiphase boundary [1], In the terminology used to describe grain boundaries, the grains on either side of this boundary can be regarded as being Σ=1-related. For the {110} interface plane, in particular, there are equal numbers of GaGa and As-As anti-site bonds across the interface. The equilibrium distance between two atoms of the same kind crossing the boundary is expected to be different from the length of normal GaAs bonds in the bulk. Therefore, the relative position of each grain on either side of an APB may be translated such that the boundary can have a lower energy situation. This translation does not affect the perfect Σ=1 coincidence site relationship. Such a lattice translation is expected for all high-angle grain boundaries as a way of relaxation of the boundary structure.

Determination of the Burgers vector of a dislocation in a Fe-Mn alloy by weak-beam image in HVEM

1978 ◽  
Vol 36 (1) ◽  
pp. 330-331
Author(s):  
Y. Ishida ◽  
H. Ishida ◽  
K. Kohra ◽  
H. Ichinose
Keyword(s):  
High Order ◽  
Simulation Technique ◽  
The Other ◽  
Image Simulation ◽  
Diffraction Vector ◽  
Burgers Vector ◽  
Weak Beam ◽  
Beam Image ◽  
Edge Component

IntroductionA simple and accurate technique to determine the Burgers vector of a dislocation has become feasible with the advent of HVEM. The conventional image vanishing technique(1) using Bragg conditions with the diffraction vector perpendicular to the Burgers vector suffers from various drawbacks; The dislocation image appears even when the g.b = 0 criterion is satisfied, if the edge component of the dislocation is large. On the other hand, the image disappears for certain high order diffractions even when g.b ≠ 0. Furthermore, the determination of the magnitude of the Burgers vector is not easy with the criterion. Recent image simulation technique is free from the ambiguities but require too many parameters for the computation. The weak-beam “fringe counting” technique investigated in the present study is immune from the problems. Even the magnitude of the Burgers vector is determined from the number of the terminating thickness fringes at the exit of the dislocation in wedge shaped foil surfaces.

Procedures for the Quantitative Determination of Autoprothrombin C

1962 ◽  
Vol 08 (03) ◽  
pp. 434-441 ◽  
Author(s):  
Edmond R Cole ◽  
Ewa Marciniak ◽  
Walter H Seegers
Keyword(s):  
Quantitative Determination ◽  
Plasma Sample ◽  
Quantitative Measure ◽  
The Other ◽  
Clotting Time ◽  
Bovine Plasma ◽  
Autoprothrombin C

SummaryTwo quantitative procedures for autoprothrombin C are described. In one of these purified prothrombin is used as a substrate, and the activity of autoprothrombin C can be measured even if thrombin is in the preparation. In this procedure a reaction mixture is used wherein the thrombin titer which develops in 20 minutes is proportional to the autoprothrombin C in the reaction mixture. A unit is defined as the amount which will generate 70 units of thrombin in the standardized reaction mixture. In the other method thrombin interferes with the result, because a standard bovine plasma sample is recalcified and the clotting time is noted. Autoprothrombin C shortens the clotting time, and the extent of this is a quantitative measure of autoprothrombin C activity.

Determination of Factor XIII Activity and of Factor XIII Inhibitors Using an Ammonium-Sensitive Electrode

1983 ◽  
Vol 50 (02) ◽  
pp. 563-566 ◽  
Author(s):  
P Hellstern ◽  
K Schilz ◽  
G von Blohn ◽  
E Wenzel
Keyword(s):  
Factor Xiii ◽  
Normal Subjects ◽  
The Other ◽  
Activity Measurement ◽  
Factor Xiii Deficiency ◽  
Assay Procedure ◽  
Stabilization Factor ◽  
Release Method ◽  
Sensitive Electrode

SummaryAn assay for rapid factor XIII activity measurement has been developed based on the determination of the ammonium released during fibrin stabilization. Factor XIII was activated by thrombin and calcium. Ammonium was measured by an ammonium-sensitive electrode. It was demonstrated that the assay procedure yields accurate and precise results and that factor XIII-catalyzed fibrin stabilization can be measured kinetically. The amount of ammonium released during the first 90 min of fibrin stabilization was found to be 7.8 ± 0.5 moles per mole fibrinogen, which is in agreement with the findings of other authors. In 15 normal subjects and in 15 patients suffering from diseases with suspected factor XIII deficiency there was a satisfactory correlation between the results obtained by the “ammonium-release-method”, Bohn’s method, and the immunological assay (r1 = 0.65; r2= 0.70; p<0.01). In 3 of 5 patients with paraproteinemias the values of factor XIII activity determined by the ammonium-release method were markedly lower than those estimated by the other methods. It could be shown that inhibitor mechanisms were responsible for these discrepancies.

THE THYMOLYTIC ACTIVITY OF 6- AND 9-HALOCORTICOIDS AND RELATED STEROIDS

1965 ◽  
Vol 49 (2) ◽  
pp. 262-270 ◽  
Author(s):  
Ralph I. Dorfman ◽  
P. G. Holton ◽  
Fred A. Kind
Keyword(s):  
Double Bond ◽  
Subcutaneous Injection ◽  
Fluocinolone Acetonide ◽  
Relative Potency ◽  
Subcutaneous Route ◽  
Adrenalectomized Rats

ABSTRACT Adrenalectomized rats were used for the determination of the relative potency of various 6- and 9-halo substituted corticoids administered subcutaneously or by gavage using thymus weightas the endpoint. By subcutaneous injection, fluocinolone acetonide was the most active corticoid at 700 times that of cortisol. This compound was also the most active corticoid by the gavage route and was judged to be 570 times as active as the standard cortisol. The introduction of the 16,17-acetonide and 16,17-acetone 21-acetate groups into 17α,21-dihydroxy-9α,11β-dichloropregna-1,4-diene-3,20-dione increased the activity by a factor of 42 and 100, respectively. The introduction of the δ1 double bond into 6α-fluoroprogesterone 16,17-acetonide caused an increase of 10-fold in thymolytic activity assessed by the subcutaneous route

EFFECT OF FEEDING ETHINYLOESTRADIOL FOR VARIOUS PERIODS BEFORE MATING ON REPRODUCTION IN THE HAMSTER

1972 ◽  
Vol 70 (3) ◽  
pp. 582-590
Author(s):  
B. K. Davis ◽  
I. Noske ◽  
M. C. Chang
Keyword(s):  
Single Dose ◽  
Pregnancy Rate ◽  
Fertility Control ◽  
Normal Pregnancy ◽  
Oestrous Cycle ◽  
The Other ◽  
Feeding Schedule ◽  
Crown Rump Length ◽  
Essentially Normal ◽  
Effect Of Feeding

ABSTRACT Ethinyloestradiol (EO) fed for various periods before mating to female hamsters affected the timing of mating and pregnancy rate. Slight effects on ovulation, foetal-crown rump length and resorption may have occurred, but effects on implantation were not apparent among pregnant hamsters. The response observed depended upon the feeding schedule adopted: hamsters fed 2.5 mg EO in a single dose, on day 3 before mating, mated normally but had a significantly lower pregnancy rate; on the other hand, animals fed 2.5 mg EO (0.21 mg/day) over three oestrous cycles, days 14–3 before mating, showed variations in the time of mating but had an essentially normal pregnancy rate; and, a group of hamsters who received the same total amount of EO (0.63 mg/day) over one oestrous cycle, days 6–3 premating, showed untowards effects by the steroid on both the timing of mating and pregnancy rate. The implications of these results are considered in relation to fertility control.

Colorimetric Determination of Amoxicillin in Pure and some Pharmaceutical Formulations Via Reaction with Potassium Permanganate as Oxidant Reagent

2019 ◽  
Vol 10 (02) ◽  
Author(s):  
Abbas Shebeeb Al-kadumi ◽  
Sahar Rihan Fadhel ◽  
Mohammed Abdullah Ahmed ◽  
Luma Amer Musa
Keyword(s):  
Potassium Permanganate ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Atomic Emission ◽  
Basic Medium ◽  
Photometric Method ◽  
Colorimetric Determination ◽  
Spectrophotometric Methods ◽  
Label Claim

We proposed two simple, rapid, and convenient spectrophotometric methods are described for the determination of Amoxicillin in bulk and its pharmaceutical preparations. They are based on the measurement of the flame atomic emission of potassium ion (in first method) and colorimetric determination of the green colored solution for manganite ion at 610 nm formed after reaction of Amoxicillin with potassium permanganate as oxidant agent (in the second method) in basic medium. The working conditions of the methods were investigated and optimized. Beer's law plot showed a good correlation in the concentration range of 5-45 μg/ml. The detection limits and relative standared deviations were (2.573, 2.814 μg/ml) (2.137, 2.498) for the flame emission photometric method and (1.844, 2.016 μg/ml) (1.645,1.932) for colorimetric methods for capsules and suspensions respectively. The methods were successfully applied to the determination of Amoxicillin in capsules and suspensions, and the obtained results were in good agreement with the label claim. No interference was observed from the commonly encountered additives and expectancies.

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