Differential-pulse polarographic determination of isonicotinic acid hydrazide,and analogous hydrazides in admixture

The differential pulse polarographic behaviour of isonicotinic, nicotinic and picolinic acid hydrazides in Britton-Robinson buffers of pH 2–11 is described. The isonicotinic compound (isoniazid) is best determined at pH 5–6 at a peak potential at ca. ?1.0 V (vs. Ag/AgCl). This method was applied to analysis of tablets. At pH 9, the peak potentials are ?1.22, ?1.34 and ?1.6 V, respectively, for the three hydrazides mentioned. Calibration graphs are linear in the range 10^?6?5×10^?4 M with relative standard deviations of 1.4–2.5%.     

Modification of Monocarboxylic Acid Hydrazides with Tropylium Salts

Russian Journal of Organic Chemistry - Nicotinic, isonicotinic, and furan-2-carboxylic acid hydrazides reacted with 2 equiv of tropylium perchlorate or tetrafluoroborate to give the corresponding...     

Hybrid compounds of <Emphasis Type="Italic">ent</Emphasis>-beyerane diterpenoid isosteviol with pyridinecarboxylic acid hydrazides. Synthesis,structure, and antitubercular activity

Hybrid compounds derived from natural diterpenoid isosteviol and antitubercular drug isoniazid (isonicotinic acid hydrazide) and its isomers (nicotinic and 2-picolinic acid hydrazides) were synthesized, and their structure in crystal and in solution was studied. The newly synthesized compounds were found to inhibit Micobacterium tuberculosis (H₃₇R_V strain) in vitro, the minimal inhibitory concentration being 10–20 μg/ml.     

Synthesis, structure and chemical transformations of 4-aminobenzaldehyde

A possibility of nucleophilic substitution of the fluorine atom in 4-fluorobenzaldehyde with amines (morpholine, piperidine or cytisine) under convection heating and microwave irradiation was shown. Reactions of 4-morpholinyl- and 4-piperidinylbenzaldehyde with hydrazides of isonicotinic and salicylic acids afford the corresponding hydrazones. The structure of the synthesized compounds was confirmed by IR, ¹H NMR spectroscopy, mass spectrometry, and X-ray analysis data.     

A Novel Method for the Rapid Determination of Isonicotinic Hydrazide in Aqueous Solutions Using Reflectance Spectrophotometry and Colorimetry

A rapid method is developed for the quantitative determination of 5–35 g/L of isonicotinic hydrazide (INH, isoniazide) in aqueous media. The method is based on the formation of copper(I) oxide in the reaction of isonicotinic hydrazide with copper ions on the surface of indicator tablets and the subsequent recording of the analytical signal by reflectance spectrophotometry and colorimetry. Aluminum oxide is proposed as a solid-phase substrate for the production of indicator tablets. Isonicotinic hydrazide can be determined in the tablet form of the Isoniazid preparation.     

The thermometric determination of isonicotinic acid hydrazide in isoniazid tablets

The determination of isonicotinic acid hydrazide in the dosage form of isoniazid tablets is done using thermometric titrimetry. The hydrazide is oxidized by hexacyanoferrate(III) ions. It is not necessary to separate the active ingredients from the powdered sample. The results from the proposed method are compared with those obtained using the standard B.P. method.     

Polarographic determination of chlorpheniramine maleate in pharmaceuticals

The electroreduction of chlorpheniramine maleate has been investigated by a.c. and d.c. polarography, coulometry and cyclic voltammetry. Polarograms recorded from 0.2 M sulphuric acid exhibit a single well-defined 2-electron wave. The current is diffusion-controlled and proportional to the concentration in the entire range 0.3–400 μg ml^?1. A simple and rapid method for the determination of chlorpheniramine maleate in tablets is described.     

Vanadametry

Summary A vanadametric method has been developed which has definite advantages over iodimetric assay and bromimetric assay for the estimation of isonicotinic acid hydrazide in tablets. The excepients such as lactose, glucose and starch do not interfere in the estimation of the hydrazide with vanadate. Unlike iodimetric and bromimetric assays, the vanadametric assay is rapid.See also Z. analyt. Chem. 160, 117 (1958).     

Simultaneous Analysis of Isoniazid and Its Impurities by CZE

An alternative methodology for simultaneous determination of isoniazid, isonicotinic acid, 4-cyanopyridine, ethyl isonicotinate and isonicotinamide by capillary zone electrophoresis, within an analysis time of 11 min, is proposed. An electrolyte composed by 50 mmol L⁻¹ of acetic acid/sodium acetate buffer and 12.5 mmol L⁻¹ of Cu²⁺, an analyte dilution in 1 mmol L⁻¹ of Brij 35 and 12.5 mmol L⁻¹ of Cu²⁺ and +20 kV voltage were optimized. After evaluating some figures of merit, such as linearity, precision, recovery and quantification limit, the method was successfully applied to the isoniazid analysis in tablets. The contents found were 99.3 mg of isoniazid and 0.3 mg of isonicotinic acid, corresponding to 0.3 % of impurity regarding the content of the active ingredient in the pharmaceutical formulation.

     

Complexation of Ni(II) with Benzoic,p-Methoxybenzoic,and Isonicotinic Acids Hydrazides in Aqueous Acetonitrile

Solvation and complexation of Ni(II) with benzoic (L¹), p-methoxybenzoic (L³), and isonicotinic (L) acids hydrazides in water and aqueous acetonitrile were studied. The coordination of acetonitrile with Ni(II) was qualitatively estimated, and the formation constant were determined for the complexes Ni(L¹)^{2 +}, Ni(L¹)2^{2 +}, Ni(L³)^{2 +}, Ni(L³)2^{2 +}, Ni(HL)^{3 +}, NiL^{2 +}, NiL(HL)^{3 +}, and NiL₂ ^{2 +}. The effects of dilution, ligand basicity, and ligand solvation on the stability of Ni(II) compounds with hydrazides of benzoic acid and its derivatives were demonstrated. The stability of the Ni(II) complexes with isonicotinic acid hydrazide is governed by dehydration of the metal ion, decrease in the donor power of the coordinating hydrazide fragment on protonation of the pyridine substituent L, formation of the intracomplex hydrogen bond between the protonated and deprotonated pyridine nitrogen atoms in NiL(HL)^{3 +}, and stacking interaction between the heterocycles in NiL₂ ^{2 +}.     

异烟酸在银溶胶上的表面增强喇曼散射及影响因素

本文研究了异烟酸吸附在银溶胶表面的表面增强喇曼散射(SERS)光谱以及卤素离子、溶液pH值及溶液浓度对异烟酸SERS光谱的影响。文章提出了离子在银溶胶表面的吸附方式,即主要以—COO~-端吸附于银溶胶表面。最后,对所述实验现象作了定性讨论。     

Electroreduction and pulse-polarographic determination of nicotinamide in multivitamin tablets

The electroreduction of nicotinamide has been investigated by d.c., a.c. and pulse polarography, cyclic voltammetry and coulometry. A single well-defined polarographic wave is obtained from 2 M sulphuric acid and from 0.1 M sodium hydroxide. In both media, nicotinamide undergoes an irreversible 2-electron reduction; 3 hydrogen ions are consumed in acidic medium and two hydrogen ions in alkaline medium. The current is diffusion-controlled and proportional to the concentration in the range 0.6–120 μg ml^?1. Reduction mechanisms are proposed. A simple and rapid method for the determination of nicotinamide in multivitamin tablets by differential pulse polarography is described.     

Indirect potentiometric determination of hydrazine, isoniazid, sulphide and thiosulphate with a chloramine-T ion-selective electrode

Indirect potentiometric procedures with chloramine-T (CAT) as the oxidant and a chloramine-T ion-selective electrode are described for the determination of hydrazine and isonicotinic acid hydrazide (isoniazid) in the 1-100 mumole range and of sulphide and thiosulphate in the 0.5-50 mumole range. The reductants react stoichiometrically with a known and excessive volume of added CAT and the unconsumed excess of CAT is measured with the CAT-selective electrode. Aqueous solutions of the reductants were analysed with an error and precision of about 1-2%. Analytical recovery of isoniazid added to tablet diluents was 97-101% (average 98.9%). Results were comparable with those obtained with a titrimetric method for the determination of isoniazid in injection solutions and tablets.     

Bench-scale biosynthesis of isonicotinic acid from 4-cyanopyridine by Pseudomonas putida

Pseudomonas putida CGMCC3830 harboring nitrilase was used in isonicotinic acid production from 4-cyanopyridine. This nitrilase showed optimum activities towards 4-cyanopyridine at pH 7.5 and 45°C. The half-life of P. putida nitrilase was 93.3 h, 33.9 h, and 9.5 h at 30°C, 38°C, and 45°C, respectively. 4-Cyanopyridine (100 mM) was fully converted into isonicotinic acid within 20 min. The bench-scale production of isonicotinic acid was carried out using 3 mg of resting cells per mL in a 1 L system at 30°C and finally, 123 g L^?1 of isonicotinic acid were obtained within 200 min without any by-products. The conversion reaction suffered from the product inhibition effect after the tenth feeding. The volumetric productivity was 36.9 g L^?1 h^?1. P. putida shows significant potential in nitrile hydrolysis for isonicotinic acid production. This paper is the first report on isonicotinic acid biosynthesis using Pseudomonas putida and it represents the highest isonicotinic acid production reported so far.     

A new synthesis of pyrazolo[1,5-d][1,2,4]triazines from pyrazolecarboxylic acid hydrazides and carbonyl compounds. I

Pyrazolo[1,5-d][1,2,4]triazines were synthesized from pyrazolecarboxylic acid hydrazides and carbonyl compounds. Pyrazolecarboxylic acid N-phenylhydrazide (1c) and formaldehyde gave not only the expected 4hn but 5 , respectively. The methyl substituted hydrazides with acetone afforded hydrazones, pyrazolotriazines or 13 depending on the position of the substituents. The reduction of both products yielded pyrazolecarboxylic acid hydrazides.     

Excellent electrocatalytic activity of benzil for direct reduction of CO_2 as well as indirect reduction of pyridine:A kinetic view of the electrocarboxylation process

Benzil,1,2-diphenylethane-1,2-dione, was used as an excellent electrocatalyst for reduction of carbon dioxide, CO_2. The reduction overpotential of CO_2 was reduced about 900 m V in the presence of a benzil mediator. The chemical reaction of the product of the electrocatalytic reduction of CO_2,(activated CO_2,CO_2~(·-)) with pyridine at a glassy carbon electrode, GCE, surface and in an acetonitrile-But_4NClO_4 solution was investigated by cyclic voltammetry, chronoamperometry and controlled potential coulometry.By chronoamperometry, the catalytic rate constant, k, for the electron transfer between benzil and CO_2 was obtained as 8.1 ± 0.4 M~(-1)s~(-1). The results indicate that pyridine has a strong interaction with the activated CO_2. The coulometry method was used to obtain the product of the pyridine chemical reaction with CO_2~(·-). The spectral characterizations of FTIR,~1H and ~(13)C NMR of the coulometry experiment product proved that the pyridine anion radical, Py~(·-), was carboxylated by CO_2~(·-), and isonicotinic acid is the final major product.     

Co(II)与烟酸类分子形成的配位聚合物的晶体结构与孔道稳定性

利用烟酸与异烟酸两种配体分别与硝酸钴在N,N'-二甲基甲酰胺(DMF)中采用溶剂热法合成了三种新的配位聚合物[CO₂(μ₂-H₂O)(nicotinic acid)₄·(DMF)] (1), [CO₂(isonicotinic acid)₄·(DMF)] (2), [Co(isonicotinicacid)₂·(DMF)] (3), 并利用单晶X射线衍射(XRD)和元素分析获得其结构信息. 通过傅里叶变换红外(FTIR)光谱、粉末X射线衍射(XRD)、热重分析(TGA)和比表面积分析等手段对结构中孔道的热稳定性进行了表征. 结果表明化合物1 具有类金刚石的拓扑结构, 结构中含有稳定的一维(1D)孔道空间. 化合物2 和3 是以异烟酸为配体, 分别在100 和160 °C下合成, 二者结构中配体以完全不同的方式与Co(II)配位, 从而使其具有不同的结构.化合物2和3的一维孔道在热处理脱附DMF分子的过程中不能稳定存在.     

Molecular ordering in isonicotinic acid on rutile TiO2(110) investigated with valence band photoemission

The adsorption of isonicotinic acid on rutile TiO(2)(110) has been investigated using synchrotron-based valence band photoemission. Structural ordering in multilayer films of the molecules is found to give rise to a strong angular dependence in the valence band intensities when measured using linearly polarized radiation. Molecular ordering in this case is proposed to be induced by intermolecular hydrogen bonding which is found to be highly dependent upon the deposition rate of the isonicotinic acid. Through comparison of the experimental data with density functional calculated valence band spectra of hydrogen-bonded isonicotinic acid molecules, we can account for the angular dependence in terms of the spatial distribution of the molecular orbitals.