Method for Trifuzol-Neo assay determination by GC-MS

2021 ◽  
pp. 4523-4528
Author(s):  
A.A. Yaroshenko ◽  
V.V. Parchenko ◽  
O.A. Bihdan ◽  
O.I. Panasenko ◽  
Yu V. Karpenko ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Quality Control ◽  
Mobile Phase ◽  
Raw Materials ◽  
Cost Effective ◽  
Scientific Interest ◽  
Research Information ◽  
Agricultural Chemistry ◽  
Derivatives Of

The derivatives of 1,2,4-triazole are of the great scientific interest in the fields of pharmaceutics, agricultural chemistry, and construction The production of Trifuzol-Neo has already been launched, and it is now commercially available. Compounds based on 1,2,4-triazole may also be useful in veterinary practice due to their antiviral activity. Trifuzol-Neo, or piperidinium ([5-(2-furanyl)-4-phenyl-4Н-1,2,4-triazol-3-yl]thio)acetate (Figure 1), has already proved to be an effective immunostimulator for poultry.Since that, the quality control of raw materials and the ready product is required during the production stage. Currently, there is only one method for determination of the assay of Trifuzol-Neo, which involves HPLC-DMD (Center of Medical Research Information and Patent and Licensing Practice of Ukraine. The main disadvantages of HPLC-DMD are the use of relatively high amounts of costly solvents (acetonitrile in this case), considerable baseline instability, and time-consuming system stabilization. Gas-chromatography is able to avoid these constrictions since it involves gas as a mobile phase, which is a more cost-effective and reproducible alternative. The newly developed GC/MS method for Trifuzol-Neo assay determination consists of the following steps: weighing 20.0mg of Trifuzol-Neo powder, dillution in 20mL methanol, injection of 0.5uL of the obtained solution to GC column (at least three times). The same operations are done with a Trifuzol-Neo standard.

A Validated Green HPTLC Method for Quantitative Determination of Dapoxetine Hydrochloride and Tadalafil in Bulk and Pharmaceutical Formulations

2020 ◽  
Vol 58 (4) ◽  
pp. 303-308 ◽  
Author(s):  
Ibrahim A Naguib ◽  
Maimana A Magdy ◽  
Basma H Anwar ◽  
Nessreen S Abdelhamid
Keyword(s):  
Quality Control ◽  
Mobile Phase ◽  
High Performance ◽  
Raw Materials ◽  
Pharmaceutical Formulations ◽  
Uv Detector ◽  
Ich Guidelines ◽  
Hptlc Method ◽  
Dapoxetine Hydrochloride

Abstract Dapoxetine hydrochloride (DAP) and Tadalafil (TAD) were separated and determined quantitatively using a validated green high-performance thin layer chromatographic (HPTLC) method in their binary mixtures either as raw materials or in pharmaceutical formulations. The concentration ranges were 0.1–1.6 and 0.2–2.5 μg/band for dapoxetine and tadalafil, respectively, with accuracies of 98.93% ± 0.62 and 99.26% ± 1.39, respectively. Silica gel HPTLC F254 plates were used to carry out the separation. The mobile phase used was a mixture of ethanol–ethyl acetate (1:9 by volume), which is environmentally green and harmless. Densitometric scanning with UV detector was used to detect the separated peaks at 222 nm. ICH guidelines were followed to validate the suggested method, and the results prove that they can be used for regular analysis in quality control laboratories with compatible results.

scholarly journals CERTIFICATION OF VEGETABLE OILS AND QUALITY CONTROL IN THE TECHNOLOGICAL PROCESS OF PRODUCTION

2019 ◽  
Vol 2019 (4) ◽  
pp. 119-126
Author(s):  
CH Bekmurotov ◽  
Keyword(s):  
Quality Control ◽  
Technological Process ◽  
Vegetable Oils ◽  
Raw Materials ◽  
Cottonseed Oil ◽  
Product Classification ◽  
Cotton Seeds ◽  
The Cost

The article reviewed the certification and quality control of the technological process for the production of vegetable oil. There is a procedure for packaging, quality control of products, determination of quality indicators and quality control of finished products. The procedure for using refined cottonseed oil and its varieties, the requirements for placement and storage of vegetable oils, as specified in the regulatory documents, the quality control of vegetable oils and other solutions for cottonseed oil are provided. The gas analyzer shows a solution for measuring the amount of solution by painting the tubes of a mixture of gas and air in oil. Detailed information on the production of vegetable oils, the cost of raw materials, the level of fat content of cotton seeds and the methods used to produce oil from cotton seeds. Methods for certification of vegetable oils, types of quality control, methods of testing and quality determination are presented. It was shown that the procedure for refined production of cottonseed oils and their types, as well as the state of the product classification of products based on the method of producing vegetable oils for consumer purposes, analysis of the sequence of refined oils and refining processes.

scholarly journals Gas-Chromatographic Determination of the Trimethylsilyl Derivatives of Polyhydric Alcohol Humectants in Tobacco and in Tobacco Smoke

1971 ◽  
Vol 6 (2) ◽  
Author(s):  
N. Carugno ◽  
S. Rossi ◽  
G. Lionetti
Keyword(s):  
Gas Chromatography ◽  
Mass Spectra ◽  
Triethylene Glycol ◽  
Chromatographic Determination ◽  
Flame Ionization ◽  
Trimethylsilyl Derivatives ◽  
Gas Chromatographic Method ◽  
Derivatives Of ◽  
Quantitative Procedure

AbstractA qualitative and quantitative procedure has been developed for the determination of humectants in manufactured tobacco by gas-chromatographic method with a flame ionization detector. It consists of extraction with methanol, concentration of the extract and treatment with Tri-Sil reagents. The operating gas-chromatographic conditions are set forth. Samples of tobacco containing glycerine, propylene glycol, diethylene glycol, triethylene glycol, 1-3 butylene glycol and sorbitol have been analysed with recoveries, for the first five ones, in the range of 95-104 %. In order to verify that each chromatographic peak corresponded to the relative glycol, with no interference by other silylated compounds, the mass spectra were obtained through the combination of gas-chromatography with mass spectrometry. The results achieved confirm, as far as tobacco is concerned, that the procedure is accurate and precise. The same method for the determination of humectants was extended to cigarette smoke. Even though this involves morecomplicated problems, as compared to tobacco, because of the presence of silylated compounds, it was found that, for certain glycols, the gas-chromatography of the trimethyl derivatives can be also used as a method of analysis. The mass spectra of some polyhydric alcohols are shown

scholarly journals Spectrodensitometric simultaneous determination of esomeprazole and domperidone in human plasma

2017 ◽  
Vol 15 (1) ◽  
pp. 293-298
Author(s):  
Pakinaz Y. Khashaba ◽  
Hassan Refat H. Ali ◽  
Mohamed M. El-Wekil
Keyword(s):  
Ethyl Acetate ◽  
Factorial Design ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
Mobile Phase ◽  
Fractional Factorial Design ◽  
Cost Effective ◽  
Fractional Factorial ◽  
Tlc Plates

AbstractA simple, rapid, cost-effective, and sensitive TLC-spectrodensitometric method for simultaneous determination of esomeprazole and domperidone was developed and tested in human plasma. Ethyl acetate: methanol: benzene: acetonitrile (5: 4: 8: 3, v/v/v/v) mobile phase was used for separation on TLC plates detected at 286 nm. The linearity ranges were 5-1200 and 2-600 ng/ spot for esomeprazole and domperidone, and limits of detection were 1.73 and 0.59 ng/spot. The effects of four variables affecting Rf were evaluated by fractional factorial design. The benzene volume and saturation time had significant effects.

scholarly journals Unusual Regularity in GC Retention of Simple Amino Acid Derivatives

2019 ◽  
Vol 6 (1) ◽  
pp. 3-14 ◽  
Author(s):  
Igor G. Zenkevich ◽  
Nino G. Todua ◽  
Anzor I. Mikaia
Keyword(s):  
Gas Chromatography ◽  
Retention Index ◽  
Methyl Esters ◽  
Elution Order ◽  
Alkyl Esters ◽  
Methyl Group ◽  
The Difference ◽  
Direct Use ◽  
Derivatives Of

Background: Application of simple regularities and general principles along with direct use of reference gas chromatography retention index data for reliable structure determination of compounds can be enhanced by determination of new regularities that are specific to certain structural elements. Objective: Revelation and interpretation of an anomaly in the elution order of alkyl esters of alkoxycarbonyl derivatives of glycine and alanine on standard and semi-standard non-polar phases. Method: Preliminary derivatization of amino acids to alkyl esters of N-alkoxycarbonyl analogs and interpretation of their gas chromatographic characteristics. Results: Alkyl esters of N-alkoxycarbonyl derivatives of alanine (Alkyl = C2H5, n- and iso-C3H7) elute prior to the same derivatives of glycine, despite the presence of an additional methyl group at C(2) in the molecule. Elution order is reversed for methyl esters of N-methoxycarbonyl derivatives. Conclusion: It is established that the peculiar behavior of alkyl esters of N-alkoxycarbonyl derivatives of glycine and alanine agrees with the concepts of gas chromatography and the known retention index regularities of organic compounds. A decrease of retention index values is a result of an introduction of an additional methyl group to a carbon atom connected to two polar fragments in a molecule like CH2XY. The dependence of the difference of retention index values for homologs of the types of CH3-CHXY and CH2XY vs. the total mass of fragments (X + Y) is similar to those for other sub-groups of analytes.

scholarly journals Recent Development of Quality Control Methods for Herbal Derived Drug Preparations

2018 ◽  
Vol 13 (12) ◽  
pp. 1934578X1801301 ◽  
Author(s):  
Gunawan Indrayanto
Keyword(s):  
Quality Control ◽  
Raw Materials ◽  
Herbal Medicines ◽  
Complex Nature ◽  
Chemical Marker ◽  
Chemical Profiling ◽  
Chemical Content ◽  
Pharmaceutical Industries ◽  
Microbial Toxins

Pharmaceutical industries should apply rigorous QC (quality control) to ensure the consistency, safety, and efficacy of their herbal derived drug-preparations. QC must be performed at every stage of the production line i.e. incoming raw materials, extractions, in-process control, finished products and keeping samples. Due to the complex nature of the chemical content of herbal drugs, two approaches to QC should be taken, that is quantitative determination of the selected marker(s) compound(s), and metabolite profiling. Contamination of herbal medicines by heavy metals, pesticides, toxic metabolites, microbial toxins, pathogenic microorganisms and other foreign matter should also be evaluated. A combination of chemical profiling and multivariate analysis (MVA) is recommended as the QC tool for the botanical identification method (BIM) of herbs, extracts, herb materials, and herbal drug preparations. Microscopic methods, DNA profiling or chemical marker(s) are not recommended for use as the sole BIM due to the lack of specificity. Only markers that meet certain criteria i.e. quality active (QA) markers can be utilized as a QC tool. The limit specification range of markers used as QC tools should be described in the analytical target profile (ATP). To gain reliable results of any analysis that has been performed at any QC laboratory, the analysis method must be validated according to the newest guidance. Sample detection limit of any toxic compound(s) should be lower than its cut-off value and MPL. The reliability of any results of analysis of a QC laboratory must be evaluated by using QC-samples for each series of measurements.

scholarly journals Scientific-methodological approach for standardization of herbal raw materials and herbal preparations using high-performance thin-layer chromatography procedure

2021 ◽  
pp. 76-89
Author(s):  
К. О. Хохлова
Keyword(s):  
Quality Control ◽  
Thin Layer ◽  
Related Species ◽  
High Performance ◽  
Raw Materials ◽  
Methodological Approach ◽  
Herbal Drugs ◽  
Closely Related Species ◽  
Layer Chromatography

The high-performance thin-layer chromatography (HPTLC) is widely used for quality control of herbal raw materials (HRM). The purpose of this work were to define the problematic issues of quality control of herbal drugs in Ukraine and to develop a systematic scientific and methodological approach for the standardization of HRM and herbal drugs using the modern analytical technique of HPTLC: to optimize the existing and develop new methods of identification and determination of adulterations, and to develop alternative methods of quantitative determination, as well as studying of the stability. As a result of a critical evaluation of existing approaches for the standardization of HRM and herbal drugs of Ukraine’s flora, numerous problematic issues were identified, including the existence of a limited number of national monographs / national parts of monographs on the HRM of the Ukraine’s flora, which were not previously standardized by other pharmacopeias; non-consideration of Ukraine’s flora species (non-pharmacopoeial) in monographs on closely related species that introduced in the State Pharmacopoeia of Ukraine; lack of specificity of combinations of physical and chemical methods used for quality control; lack of specificity and reproducibility, the labor intensity of methods; necessity of usage of toxic solvents and precursors; use of different groups of markers and methods for the HRM and its finished product or HRM and its closely related species, etc. The proposed systematic scientific and methodological approach includes: a preliminary collection of information about the object of study, markers/groups of bioactive substances, approaches to its standardization; theoretical evaluation of existing techniques of quality control in monographs on HRM and experimental approbation using samples of domestic plants, determination of the need for optimization of existed methods by the parallel development of specific, reproducible and documented methods for identification, adulterations’ detection, quantification, and bio-detection (if necessary) by HPTLC method. The approach is illustrated with examples. The proposed approach can be used for comprehensive HPTLC analysis of domestic HRM and herbal drugs for research, prevention of adulteration, standardization of initial HRM and its finished product, pharmaceutical development, and stability studies.

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