scholarly journals A Simple and Sensitive Inhibitory Kinetic Method for the Carbocisteine Determination

2021 ◽  
Vol 66 (1) ◽  
Author(s):  
Abhishek Srivastava ◽  
Vivek Sharma ◽  
Vinay Kumar Singh ◽  
Krishna Srivastava
Keyword(s):  
Good Accuracy ◽  
Quantitative Estimation ◽  
Kinetic Method ◽  
Fixed Time ◽  
Disodium Salt ◽  
Disulfonic Acid ◽  
Stable Complex ◽  
Reaction Conditions ◽  
Kinetic Determination

Abstract. A fast, reproducible, and sensitive method is proposed for the kinetic determination of carbocisteine (CCys). The method depends on the inhibitory property of carbocisteine, which reduces the Hg2+ catalyzed substitution rate of cyanide from [Ru(CN)6]4- with N-R-salt (1-Nitroso-2-naphthol-3,6-disulfonic acid disodium salt) via forming a stable complex with Hg2+. Spectrophotometric measurements were carried out by recording the absorbance at 525 nm (λmax of [Ru(CN)5 Nitroso-R-Salt]3- complex) at a fixed time of 10 and 15 min under the optimized reaction conditions with [N-R-salt] = 4.5 × 10-4 M, I = 0.05 M (KNO3), Temp = 45.0 ± 0.2 o C, pH = 7.0 ± 0.03, [Hg2+] = 8.0 × 10-5 M and [Ru(CN)64-] = 4.25 × 10-5  M. With the proposed method, CCys can be determined quantitatively down to 3.0 × 10-6 M. This methodology can be effectively used for the rapid quantitative estimation of CCys in the pharmaceutical samples with good accuracy and reproducibility. The addition of common excipients in pharmaceuticals even up to 1000 times with [CCys] does not interfere significantly in the estimation of CCys.   Resumen. Se propone un método rápido, reproducibley sensible para la determinación cinética de la carbocisteina (CCys). El método depende de la propiedad inhibitoria de la carbocisteina que reduce la tasa de sustitución catalizada por Hg2+ del cianuro de [Ru(CN)6]4- con la sal N-R (sal disódica del ácido 1-Nitroso-2-naftol-3,6-disulfónico) mediante la formación de un complejo estable con Hg2+. Las mediciones espectrofotométricas se llevaron a cabo registrando la absorbancia a 525 nm (λmax del complejo [Ru(CN)5 Sal-Nitroso-R]3-) en un tiempo fijo de 10 y 15 min en las condiciones de reacción optimizadas con [sal-NR] = 4.5 × 10-4 M, I = 0.05 M (KNO3), Temp = 45.0 ± 0.2 o C, pH = 7.0 ± 0.03, [Hg2+] = 8.0 × 10-5 M y [Ru(CN)64-] = 4.25 × 10-5 M. Con el método propuesto, CCys se puede determinar cuantitativamente hasta 3,0 × 10-6 M. Esta metodología se puede utilizar eficazmente para la estimación cuantitativa rápida de CCys en las muestras farmacéuticas con buena precisión y reproducibilidad. La adición de excipientes comunes en productos farmacéuticos incluso hasta 1000 veces con [CCys] no interfiere significativamente en la estimación de CCys.

scholarly journals Quantitative Estimation of D-Penicillamine in Pure and Pharmaceutical Samples Using Inhibitory Kinetic Spectrophotometric Method

2020 ◽  
Vol 11 (4) ◽  
pp. 11404-11417
Keyword(s):  
Quantitative Estimation ◽  
Catalytic Efficiency ◽  
Bioactive Molecules ◽  
Stable Complex ◽  
Kinetic Measurements ◽  
Kinetic Determination ◽  
Pharmaceutical Samples ◽  
Optimum Reaction ◽  
Kinetic Spectrophotometric

Sulfur is the key element in a large number of drugs and bioactive molecules. Organo-sulfur compounds inhibit the catalytic efficiency of Hg2+ by forming a stable complex with it. The Hg2+ catalyzed exchange rate of cyanide with pyrazine from [Ru(CN)6]4- will be reduced by the addition of the sulfur-containing drug, D-penicillamine (D-PCN). This inhibitory property of D-PCN can be employed for its micro-level kinetic determination. Optimum reaction condition viz. Temperature = 45.0 ± 0.1 o C, I = 0.1 M (KCl), [Hg+2] = 1.5 × 10-4 M, [pyrazine] = 7.5 × 10-4 M, pH = 4.0 ± 0.02, and [Ru(CN)64-] = 5.25 × 10-5 M were utilized to investigate the kinetic measurements at 370 nm (λmax of [Ru(CN)5 Pz]3- complex). To acknowledge the inhibition induced by D-PCN on Hg2+ catalyzed substitution of cyanide with pyrazine from [Ru(CN)6]4-, a modified mechanistic scheme has been proposed. D-PCN can be quantitatively determined up to 1.0 × 10-6 M level by the proposed analytical method. The methodology can be economically and effectively employed for the quantitative determination of D-PCN in different samples. This methodology can also be convincingly adopted for the quick determination of D-PCN in the pharmaceutical samples with good accuracy and reproducibility. The addition of common excipients in pharmaceuticals even up to 1000 times with [D-PCN] does not interfere significantly in the estimation of D-PCN.

scholarly journals Kinetic determination of As(III) in solution

2003 ◽  
Vol 68 (10) ◽  
pp. 765-769
Author(s):  
Sofija Rancic ◽  
Rangel Igov ◽  
Todor Pecev
Keyword(s):  
Acid Solution ◽  
Relative Error ◽  
Reaction Rate ◽  
Kinetic Method ◽  
Kinetic Equations ◽  
Strong Acid ◽  
Kinetic Determination

A new reaction is suggested and a new kinetic method is elaborated for the As(HI) traces determination in solution, on the basis of their catalyzing effect on komplexon III (EDTA) oxidation by KMnO4 in a strong acid solution (H2SO4). Using a spectrophotometric technique, a sensitivity of 72 ng/cm3 As(IIl) was achieved. The relative error of method varies from 5.5 to 13.9 % for As(HT) concentration range from 83 to 140 ng/cm-1. Appropriate kinetic equations are formulated and the influence of some other ions, including the As(V), upon the reaction rate is tested.

Automated kinetic determination of lactate dehydrogenase isoenzymes in serum.

1977 ◽  
Vol 23 (10) ◽  
pp. 1928-1930 ◽  
Author(s):  
L H Bernstein
Keyword(s):  
Lactate Dehydrogenase ◽  
Kinetic Method ◽  
Previous Method ◽  
Kinetic Determination ◽  
Steady State Kinetic ◽  
Enzyme Subunits ◽  
Isoenzyme Composition ◽  
State Kinetic ◽  
Lactate Dehydrogenase Isoenzymes

Abstract A steady-state kinetic method has been revised for measuring lactate dehydrogenase isoenzyme activities, which relates the inhibition of heart-type isoenzyme activity to the overall isoenzyme composition of the enzyme subunits. The method depends on the pH-dependent formation of an inhibitory ternary complex by the heart-type isoenzyme with NAD+ and pyruvate (if the reaction is measured by NADH oxidation). A preincubation step in the previous method is eliminated. The isoenzymes are measured by measuring the reduction of pyruvate in two different concentrations, which favor either the total or fractional activity, depending on the concentrations of pyruvate and the percentage of heart-type subunits. The method has been adapted to a centrifugal analyzer, which has speeded automated isoenzyme determinations, with an accuracy comparable to that for electrophoretic methods.

Kinetic study of the Jaffé reaction for quantifying creatinine in serum: 2. Evaluation of buffered reagent and comparison of different data-processing options.

1989 ◽  
Vol 35 (3) ◽  
pp. 360-363 ◽  
Author(s):  
B L Bacon ◽  
H L Pardue
Keyword(s):  
Data Processing ◽  
Curve Fitting ◽  
Fixed Time ◽  
Good Precision ◽  
Creatinine Concentration ◽  
Kinetic Determination ◽  
Predictive Method ◽  
Target Values ◽  
Standard Additions

Abstract Here we describe the evaluation of several data-processing options for the kinetic determination of creatinine by use of the Jaffé reaction. Data-processing options evaluated include initial-rate, two-point fixed-time, rate at t = k-1, and multipoint curve-fitting predictive methods. We evaluated these options for a buffered formulation of the Jaffé reagent and studied the effects of potential interferents, including glucose, acetoacetate, bilirubin, and albumin, on each option. To reduce effects of bilirubin, we evaluated the inclusion of a preoxidation step with ferricyanide. All the data-processing options gave good precision and linearity between the measurement objective and creatinine concentration. However, differences between slopes of calibration plots in aqueous and serum matrices ranged from a high of +60% for the two-point, fixed-time method to a low of -11% for the curve-fitting, predictive method. Standard additions of creatinine to sera were quantified reliably (yielding 96% to 102% of target values) by the predictive method and less reliably (62% to 102%) by the other methods. We conclude that the predictive method has the potential to yield the most reliable results for creatinine.

scholarly journals Photometric determination of aqueous cobalt (II), nickel (II), copper (II) and iron (III) with 1-nitroso-2-naphthol-3,6-disulfonic acid disodium salt in gelatin films

2012 ◽  
Vol 10 (5) ◽  
pp. 1617-1623 ◽  
Author(s):  
Elena Reshetnyak ◽  
Nataliia Ivchenko ◽  
Nataliya Nikitina
Keyword(s):  
Metal Complexes ◽  
Simultaneous Determination ◽  
Isoelectric Point ◽  
Electrostatic Interaction ◽  
Photometric Determination ◽  
Disodium Salt ◽  
Photographic Film ◽  
Disulfonic Acid ◽  
Gelatin Films

AbstractPhotometric determination of aqueous Co(II), Cu(II), Ni(II) and Fe(III) was performed using indicator films prepared by immobilization of 1-nitroso-2-naphthol-3,6-disulfonic acid disodium salt (NRS) into hardened photographic film. Immobilization was based on electrostatic interaction of reagent and metal complexes with the gelatin. The isoelectric point pH of hardened gelatin (4.46±0.04) was evaluated by viscometry. Co(II), Fe(III), Ni(II) form 1:3 complexes with NRS in gelatin at pH 2 and Cu(II) forms 1:2 complexes. Their log β′ values were: Co-6.7, Fe-8.6, Cu-8.0, and Ni-6.4. The absorption maxima were: 370nm for NRS, and 430nm, 470nm, 495nm and 720nm for complexes of Co(II), Ni(II), Cu(II) and Fe(III). An algorithm for their simultaneous determination using the indicator films was developed. The detection limits were: clim(Co2+) = 0.45×10−5 M, clim(Fe3+) = 0.50×10−5 M, clim(Cu2+) = 0.67×10−5 M, clim(Ni2+) = 0.75×10−5 M,; and their sum clim(ΣMn+) = 0.82×10−5 M.

scholarly journals Kinetic Spectrophotometric Determination of Gemifloxacin Mesylate and Moxifloxacin Hydrochloride in Pharmaceutical Preparations Using 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole

2014 ◽  
Vol 2014 ◽  
pp. 1-12 ◽  
Author(s):  
Mohammed G. Abdel Wahed ◽  
Ragaa El Sheikh ◽  
Ayman A. Gouda ◽  
Sayed Abou Taleb
Keyword(s):  
Limit Of Detection ◽  
Kinetic Method ◽  
Pharmaceutical Preparations ◽  
Fixed Time ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Significant Difference ◽  
Kinetic Spectrophotometric ◽  
Comparison Of The Results

Simple, sensitive, and accurate kinetic spectrophotometric method was proposed for the determination of gemifloxacin mesylate (GMF) and moxifloxacin hydrochloride (MOX) in pure forms and pharmaceutical preparations (tablets). The method is based on coupling the studied drugs with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) in the presence of alkaline borate buffer. Spectrophotometric measurement was achieved by recording the absorbance at 466 and 464 nm for GMF and MOX, respectively, after a fixed time of 20 and 15 min on a water bath adjusted at 70 ± 5°C for both drugs. The different experimental parameters affecting the development and stability of the color were carefully studied and optimized. The absorbance-concentration plots were linear over the ranges 0.5–8.0 and 2.0–12 μg mL−1for GMF and MOX, respectively. The limit of detection of the kinetic method was about 0.12 (2.47 × 10−7 M) and 0.36 (8.22 × 10−7 M) μg mL−1for GMF and MOX, respectively. The proposed methods have been applied and validated successfully with percentage relative standard deviation (RSD% ≤ 0.52) as precision and percentage relative error (RE% ≤ 1.33) as accuracy. The robustness of the proposed method was examined with recovery values that were 97.5–100.5 ± 1.3–1.9%. Statistical comparison of the results with the reference spectrophotometric methods shows excellent agreement and indicates no significant difference in accuracy or precision.

scholarly journals Pulse perturbation technique for determination of piroxicam in pharmaceuticals using an oscillatory reaction system

2013 ◽  
Vol 11 (2) ◽  
pp. 180-188 ◽  
Author(s):  
Nataša Pejić ◽  
Nataša Sarap ◽  
Jelena Maksimović ◽  
Slobodan Anić ◽  
Ljiljana Kolar-Anić
Keyword(s):  
Perturbation Technique ◽  
Kinetic Method ◽  
Reaction System ◽  
Direct Determination ◽  
Pharmaceutical Formulations ◽  
Oscillatory Reaction ◽  
Reaction Conditions ◽  
Good Sample ◽  
Pulse Perturbation

AbstractA simple and reliable novel kinetic method for the determination of piroxicam (PX) was proposed and validated. For quantitative determination of PX, the Bray-Liebhafsky (BL) oscillatory reaction was used in a stable non-equilibrium stationary state close to the bifurcation point. Under the optimized reaction conditions (T = 55.0°C, [H2SO4]0 = 7.60×10−2 mol L−1, [KIO3]0 = 5.90×10−2 mol L−1, [H2O2]0 = 1.50×10−1 mol L−1 and j 0 = 2.95×10−2 min−1), the linear relationship between maximal potential shift ΔE m , and PX concentration was obtained in the concentration range 11.2–480.5 µg mL−1 with a detection limit of 9.9 µg mL−1. The method had a rather good sample throughput of 25 samples h−1 with a precision RSD = 4.7% as well as recoveries RCV ≤ 104.4%. Applicability of the proposed method to the direct determination of piroxicam in different pharmaceutical formulations (tablets, ampoules and gel) was demonstrated.

scholarly journals Analytical application of acidic victoria blue 4R mixture with KBrO3 for the kinetic determination of traces of antimony(III) by spectrophotometry

2012 ◽  
Vol 31 (1) ◽  
pp. 29
Author(s):  
Violeta Mitić ◽  
Snežana Nikolić-Mandić ◽  
Vesna Stankov-Jovanović
Keyword(s):  
Reaction Rate ◽  
Kinetic Method ◽  
Operating Conditions ◽  
Rate Equations ◽  
Optimum Operating ◽  
Acid Media ◽  
Kinetic Determination ◽  
Hydrochloric Acid Media ◽  
Optimized Conditions

The present paper describes a simple, selective and sensitive kinetic method for the determination of trace amounts of Sb(III) in the presence of Sb(V) based on its inhibition effect on the redox reaction between bromate and Victoria blue 4R (V.B. 4-R) in hydrochloric acid media. The reaction was followed spectrophotometrically by measuring the decrease in the absorbance of V.B. 4-R at 596.3 nm. Optimum operating conditions regarding reagent concentrations were established. The optimized conditions yielded a theoretical detection limit of 1.30·10‒8 g cm–3 Sb(III) based on the 3S0 criterion. The method allows the determination of Sb(III) in the range of 5·10‒8 ‒ 1.1·10‒6 g cm–3. The effects of certain foreign ions the reaction rate were determined for an assessment of the selectivity of the method. The kinetic parameters of the reaction were reported, and the rate equations were suggested. The results were validated statistically and through recovery studies. The proposed method has been successfully applied to the determination of Sb(III) in various model and real samples.

scholarly journals Spectrophotometric Determination of Praseodymium by 1,4- Dihydroxyanthraquinone after its Selective Separation from Rosetta Monazite Rare Earth Concentrate by Solvent Extraction

2015 ◽  
Vol 1 (2) ◽  
Author(s):  
Abdel Fattah N. A   -      a Sadeek A. S    -      b Ali B.
Keyword(s):  
Rare Earth ◽  
Good Accuracy ◽  
Molar Absorptivity ◽  
Selective Separation ◽  
Air Oxidation ◽  
Reaction Conditions ◽  
Relative Standard ◽  
Colour Development ◽  
Sensitive Spectrophotometric Method

A rare earths concentrate of Rosetta monazite assays about 44, 23, 16.94 and 5.91 % for Ce, La, Nd and Pr respectively. Separation of cerium by air oxidation at 200oC. Selective separation of Pr by D2EHPA at pH1 followed by a sensitive spectrophotometric method which described for the determination of praseodymium (Pr) with l,4-dihydroxyanthraquinone . The calibration curve was linear from   0.1 to 12 µgml -1 praseodymium. The influences of various parameters and reaction conditions for maximum colour development were investigated. The relative standard deviation for determination of 1 µgml-1 praseodymium has found to be 1.3 after 5 repeated determinations; percent error 5.02%, molar absorptivity (ε) was 1.23x106M-1 cm-1and detection limit was 0.1µgml-1. The method for determination of praseodymium showed good accuracy and selectivity.

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