The use of photogenerated iodine in determination of the dibazol content in solid and liquid dosage formulations

2021 ◽  
Vol 87 (2) ◽  
pp. 19-24
Author(s):  
E. V. Turusova
Keyword(s):  
Generation Time ◽  
Quantitative Estimation ◽  
Potato Starch ◽  
Analytical Signal ◽  
Acetate Buffer Solution ◽  
Molar Ratio ◽  
Buffer Solution ◽  
Solution Ph ◽  
Solid Dosage

A rapid method for the determination of Dibazol (bendazol hydrochloride) in liquid and solid dosage forms (DF) has been developed. The method is based on converting the drug into an analytical form and titrating the physiologically active compound (PAC) with a solution of photogenerated iodine obtained by irradiation of an auxiliary solution containing potassium iodide, a mixture of sensitizers (sodium eosinate: fluorescein: auramine, taken in a molar ratio of 1:1:1) and an acetate buffer solution (pH 5.6). A decrease in the titrant content in the cell due to interaction with Dibazol was recorded by a decrease in the current in the amperometric circuit. Stabilization of the current in the circuit indicated the completeness of the reaction, thus providing for estimation of the PAC content in a DF. Further irradiation of the solution and measurement of the generation time required to replenish the titrant loss in the cell also ensure the quantitative estimation of the PAC content in the preparation. The method has been tested on solid dosage form and sterile solutions of Dibazol intended for intramuscular and intravenous administration. A slight effect of stabilizers (hydrochloric acid, ethanol) and auxiliary substances (potato starch) present in the DF on the photogeneration of the titrant was observed. The determined Dibazol content in solid and liquid DF falls within the range recommended by the order of the Ministry of Health of the Russian Federation (26.10.2015 No. 751n) and OFS.1.4.2.0009.15, which indicates that the quality of the drug meets the GMP standards. The linear dependence of the analytical signal on the Dibazol concentration is observed in the range of 13.5 – 134.7 mg for the drug «Dibazol-UBF, tablets, 20 mg». The calculated limits of Dibazol detection and quantitative determination by changes in the current strength and generation time are (4.71; 3.56) and (14.26; 10.77) mg, respectively. The use of developed technique in the analysis of drugs containing Dibazol reduces both the time of single determination due to the absence of the need for standardization of solutions, and the cost of a single analysis, since it does not require the use of expensive equipment and reagents.

The use of photogenerated iodine for the determination of isoniazid in solid dosage formulation

2021 ◽  
Vol 87 (3) ◽  
pp. 5-10
Author(s):  
E. V. Turusova ◽  
O. E. Nasakin ◽  
A. N. Lyshchikov
Keyword(s):  
Active Compound ◽  
Potato Starch ◽  
Phosphate Buffer Solution ◽  
Analytical Signal ◽  
Molar Ratio ◽  
Buffer Solution ◽  
Solution Ph ◽  
Solid Dosage ◽  
Dosage Formulation

A shot cut method for the determination of isoniazid in a solid dosage formulation (DF) has been developed. The method is based on isoniazid titration with a solution of photogenerated iodine obtained as a result of irradiation of an auxiliary solution containing potassium iodide, a mixture of sensitizers (sodium eosinate, fluorescein, auramine taken in a molar ratio of 1:1:1) and phosphate buffer solution (pH 7.5). Since the titrant content in the cell was controlled using the voltammetric method (amperometric titration with two polarized electrodes), the interaction of a physiologically active compound with the latter was accompanied by a decrease in the amount of titrant in the cell and, hence, in the current in amperometric circuit. Stabilization of the current in the circuit of the amperometric setup indicated the completeness of the reaction, and, therefore, provided estimation of the content of a physiologically active compound in the dosage formulation. Further irradiation of the solution and measurement of the generation time required to replenish the loss of titrant in the cell also made it possible to regulate the content of isoniazid in the preparation. The technique was tested on the samples of solid dosed formulations. It was shown that the components of the tablet mass (calcium stearate monohydrate, polysorbate, crospovidone and potato starch) do not affect the results of the determination of physiologically active compound provided that the analyzed form is obtained at room temperature. The determined content of isoniazid in a solid dosage formulation varies in the range of 286.0 – 296.0 mg and falls within the range recommended by the General Pharmacopoeia Monograph 1.4.2.0009.15 (285 – 315 mg), which indicates that the quality of the drug meets the GMP standards. The linear dependence of the analytical signal on the concentration of physiologically active compound is observed in the range of 161 – 1610 mg for the drug «Isoniazid. Tablets, 300 mg». The calculated detection limits and quantitative determination are 13.5 and 41.0 mg (both in terms of change in the current strength and in the time of titrant generation), respectively. The developed photochemical method for the determination of isoniazid in solid dosed formulation is easy to use, meets the requirements set out in the guidelines for validation of bioanalytical methods, and does not require expensive equipment. The method can be recommended for routine control of the DF quality indicators in any analytical laboratory.

Capillary isotachophoresis of piperidinoethylethers of the alkoxyphenylcarbamic acids

1986 ◽  
Vol 51 (5) ◽  
pp. 993-1000 ◽  
Author(s):  
Zdeněk Chmela ◽  
Jozef Čižmárik ◽  
Zdeněk Stránský
Keyword(s):  
Acid Medium ◽  
Steric Hindrance ◽  
Acetate Buffer ◽  
Acetate Buffer Solution ◽  
Capillary Isotachophoresis ◽  
Buffer Solution ◽  
Solution Ph ◽  
Successful Separation

Conditions for the separation and determination of N-[2-(alkoxyphenylcarbamoyloxy)-ethyl]-piperidinium chlorides ( analogues of heptacaine) by the capillary isotachophoresis have been studied. For the successful separation of lower alkoxy derivatives the acetate buffer solution, pHL = 4.75, was found to be a suitable leading electrolyte (K+ as the leading ion) and β-alanine a suitable terminator. The separation can be achieved even in the acid medium with H+ as the leading ion and with a voluminous terminating cation. For instance, pseudoaconitine or N-[2-(2-heptyloxyphenylcarbamoyloxy)-ethyl]-benzylpiperidinium chloride were found to be acceptable. The steric hindrance of the solvation, characteristic for 2-alkoxy isomers, makes their separation from 3- or 4-alkoxy isomers possible, with the exception of methoxy derivatives.

Liquid Chromatographic Determination of Taurine in Vitamin Premix Formulations

1987 ◽  
Vol 70 (5) ◽  
pp. 799-801
Author(s):  
Gowdahalli N Subba Rao
Keyword(s):  
Internal Standard ◽  
Aminocaproic Acid ◽  
Chromatographic Determination ◽  
Acetate Buffer Solution ◽  
Precolumn Derivatization ◽  
Buffer Solution ◽  
Solution Ph ◽  
Bicarbonate Buffer ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method is described for the determination of taurine in vitamin and vitamin-mineral premix formulations. The method involves extraction of taurine with 0.1 M bicarbonate buffer, followed by precolumn derivatization with dansyl chloride and LC using fluorescence detection. 6-Aminocaproic acid is used as an internal standard. A reverse phase analytical column and a mobile phase of 0.1M acetate buffer solution (pH 7.2)-acetonitrile (75 + 25) are used. Vitamins, minerals, and other excipients in the premix formulations do not interfere in the determination. The method is simple, precise, and accurate

Thioglycolic acid capped CdS quantum dots as a fluorescent probe for the nanomolar determination of dopamine

2015 ◽  
Vol 7 (16) ◽  
pp. 6791-6798 ◽  
Author(s):  
Anuja Elevathoor Vikraman ◽  
Ammu Rosin Jose ◽  
Meera Jacob ◽  
Krishnapillai Girish Kumar
Keyword(s):  
Quantum Dots ◽  
Fluorescent Probe ◽  
Thioglycolic Acid ◽  
Acetate Buffer ◽  
Acetate Buffer Solution ◽  
Cds Quantum Dots ◽  
Buffer Solution ◽  
Solution Ph ◽  
Selective Determination

Thioglycolic acid (TGA) capped CdS quantum dots (QDs) have been successfully employed as an efficient nano sized fluorescent probe for the selective determination of dopamine (DA) in acetate buffer solution (pH 7).

Development and Validation of Stability Indicating HPLC Method for the Determination of Impurities in the Sterile Mixture of Cefoperazone and Sulbactam

2019 ◽  
Vol 15 (7) ◽  
pp. 762-775
Author(s):  
Ramu Ivaturi ◽  
Thuttagunta Manikya Sastry ◽  
Satyaveni Sunkara
Keyword(s):  
Quantitative Estimation ◽  
Ammonium Hydroxide ◽  
Hplc Method ◽  
Forced Degradation ◽  
Buffer Solution ◽  
Solution Ph ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Validation Parameters ◽  
Abdominal Infections

Background: Cefoperazone Sulbactam injection is a cephalosporin antibiotic with a β- lactamase inhibitor used in the treatment for intra abdominal infections, Urinary track infections, surgical infections, etc. The combination is not official in any of the pharmacopeia for their content and impurities determination. Introduction: The present study involves the development of a simple, rapid, accurate, sensitive and stability indicating RP-HPLC method for the quantitative estimation of Cefoperazone Sulbactam mixture and its impurities in bulk and pharmaceutical dosage forms. Methods: 0.005 M Tetrabutyl ammonium hydroxide buffer solution pH adjusted to 6.80 and Acetonitrile combination has been used in a gradient programme with a flow rate of 1.0 ml/min. The retention time of Cefoperazone and Sulbactam were observed at around 8.5 and 19.5 minutes respectively. The UV detection was carried out at a wavelength of 230 nm. The chromatographic separation was achieved using Waters xbridge C18-150*4.6 mm, 3.5 µm HPLC column. The method has been validated according to the current International Council for Harmonization (ICH) guidelines for the method validation parameters such as Specificity, linearity, range, accuracy, precision, robustness and sensitivity. Results: The validation results indicate that the method is specific, as the known impurities and other impurities formed during the forced degradation studies were not co-eluting with the main components. Moreover, all these impurities were found to be spectrally pure, proving the stability indicating power of the method. The linearity and range of the method is in the range of 0.01-150%, highly accurate (100.2%), precise (<1%) and robust. Conclusion: The proposed method was accurate and specific for the quantitative analysis of Cefoperazone and Sulbactam and their related impurities in the sterile mixture. Hence the proposed method can be used for the quantification of impurities in routine as well as stability analysis in the development as well as quality control laboratories.

Non-enzymatic determination of purine nucleotides using a carbon dot modified glassy carbon electrode

2019 ◽  
Vol 11 (30) ◽  
pp. 3866-3873 ◽  
Author(s):  
R. Karthikeyan ◽  
D. James Nelson ◽  
S. Abraham John
Keyword(s):  
Glassy Carbon ◽  
Low Cost ◽  
Phosphate Buffer Solution ◽  
Purine Nucleotides ◽  
Buffer Solution ◽  
Solution Ph ◽  
Carbon Dot ◽  
Enzymatic Determination ◽  
Sensitive Determination

Selective and sensitive determination of one of the purine nucleotides, inosine (INO) using a low cost carbon dot (CD) modified glassy carbon (GC) electrode in 0.2 M phosphate buffer solution (pH 7.2) was demonstrated in this paper.

Polarographic Determination of Zinc in Compounded Rubber

1950 ◽  
Vol 23 (4) ◽  
pp. 975-980
Author(s):  
F. C. J. Poulton ◽  
L. Tarrant
Keyword(s):  
Zinc Oxide ◽  
Ammonium Acetate ◽  
Potassium Thiocyanate ◽  
Acetate Buffer Solution ◽  
Acid Electrolyte ◽  
Buffer Solution ◽  
Ammonium Acetate Buffer ◽  
Ammonium Acetate Buffer Solution ◽  
Gravimetric Procedure

Abstract Reasons are advanced for the unsatisfactory nature of some of the older methods for the determination of very small amounts of zinc in compounded rubber, particularly in latex mixings. The polarographic technique offers a possible solution, but most of the commoner electrolytes for the electroreduction of this metal are alkaline, and give rise to similar errors as are met in the gravimetric procedure. The development of a suitable acid electrolyte was therefore undertaken, and ways of dealing with likely interferences were examined. The electroltye finally recommended is a potassium thiocyanate-ammonium acetate buffer solution; iron, when present, is reduced to the ferrous condition by potassium iodide. The method was used to determine zinc oxide in a series of mixings of known composition ranging from 0.8 to 40 per cent. In all except the highest proportions of zinc oxide, the figures obtained agree well with the theoretical.

Study on the Inclusion Behavior of Cucurbit [n] uril with Phenylalanine

2011 ◽  
Vol 197-198 ◽  
pp. 1153-1156
Author(s):  
Ning Chen ◽  
Ya Bin Li
Keyword(s):  
1H Nmr ◽  
Interaction Mechanism ◽  
Acetate Buffer Solution ◽  
Molar Ratio ◽  
High Concentration ◽  
Buffer Solution ◽  
Visible Absorption ◽  
Nmr Spectrum ◽  
Application Range ◽  
Uv Visible

The characteristics of host-guest complexes between cucurbit[n]uril (CB [n]) and phenylalanine were investigated by UV-visible absorption spectroscopy in acetate buffer solution at room temperature. It was found that the UV-visible absorption increased steadily with constantly dropping the high concentration of cucurbit[6]uril (CB [6]) and cucurbit[8]uril (CB [8]) in the phenylalanine solution which indicates that there are some interaction betweenCB [n] and phenylalanine.Then CB [6] and phenylalanine at molar ratio of 1:1 to weigh while CB [8] and phenylalanine at molar ratio of 1:2, respectively, are both demonstrated by 1H NMR spectra. 1H NMR spectrum of complexes was obtained, indicating an enthalpic driving force for host-guest complexes. The possible interaction mechanism and inclusion mode were also discussed. This work may extend the application range of CB [n] in supramolecular and pharmaceutical analysis.

scholarly journals New Spectrophotometric Method for Determination of Cadmium

2009 ◽  
Vol 6 (s1) ◽  
pp. S496-S500
Author(s):  
K. S. Parikh ◽  
R. M. Patel ◽  
K. N. Patel
Keyword(s):  
Stability Constant ◽  
Spectrophotometric Method ◽  
Basic Medium ◽  
Buffer Solution ◽  
Solution Ph ◽  
Yellow Colour ◽  
Maximum Absorbance ◽  
The Stability

The reagent 2-hydroxy-4-n-butoxy-5-bromopropiophenone thiosemicarbazone (HBBrPT) has been used for the determination of Cd(II) by using spectrophotometric method. The reagent HBBrPT gave an intense yellow colour with Cd(II) solution in basic medium. The maximum absorbance was observed at 440 nm, in basic buffer solution (pH 10.00). The molor absorptivity and Sandell’s sensitivity of Cd(II)-HBBrPT complex were 4035 mol-1cm-1and 0.02765 μg cm-2respectively. The stability constant of 1:2 Cd(II)-HBBrPT complex was 8.46×106. The effect of various iron was also studied.

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