scholarly journals Current Methods for the Extraction and Analysis of Isothiocyanates and Indoles in Cruciferous Vegetables

Analytica ◽  
2021 ◽  
Vol 2 (4) ◽  
pp. 93-120
Author(s):  
Sofia Karanikolopoulou ◽  
Panagiota-Kyriaki Revelou ◽  
Marinos Xagoraris ◽  
Maroula G. Kokotou ◽  
Violetta Constantinou-Kokotou
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Analytical Techniques ◽  
Extraction Methods ◽  
Analytical Determination ◽  
Cruciferous Vegetables ◽  
Plant Metabolites ◽  
Secondary Plant Metabolites ◽  
Wide Range

Cruciferous vegetables are characterized by the presence of sulfur-containing secondary plant metabolites known as glucosinolates (GLS). The consumption of cruciferous vegetables such as broccoli, cabbage, rocket salad, and cauliflower has been related to the prevention of non-communicable diseases. Their beneficial effects are attributed to the enzymatic degradation products of GLS, e.g., isothiocyanates and indoles. Owing to these properties, there has been a shift in the last few years towards the research of these compounds and a wide range of methods for their extraction and analytical determination have been developed. The aim of this review is to present the sample preparation and extraction procedures of isothiocyanates and indoles from cruciferous vegetables and the analytical methods for their determination. The majority of the references that have been reviewed are from the last decade. Although efforts towards the application of eco-friendly non-conventional extraction methods have been made, the use of conventional solvent extraction is mainly applied. The major analytical techniques employed for the qualitative and quantitative analysis of isothiocyanates and indoles are high-performance liquid chromatography and gas chromatography coupled with or without mass spectrometry detection. Nevertheless, the analytical determination of isothiocyanates presents several problems due to their instability and the absence of chromophores, making the simultaneous determination of isothiocyanates and indoles a challenging task.

scholarly journals Analytical control optimization of residues fungicides from the class of pyrazole carboxamides in water

2017 ◽  
Author(s):  
A. M. Antonenko ◽  
O. M. Korshun ◽  
D. S. Mіlokhov ◽  
A. О. Lipavska ◽  
T. V. Ruda ◽  
...  
Keyword(s):  
High Performance ◽  
World Market ◽  
Analytical Determination ◽  
Analytical Control ◽  
Chromatography Method ◽  
Bidistilled Water ◽  
Wide Range ◽  
The World ◽  
Liquid Chromatography Method

Introduction. Over the past few years, fungicidal formulations based on fluxapyroxad, penthiopyrad, isopyrazam and sedaxan have been proposed in the world market. Such pesticides meet modern requirements and are recommended in the world to protect more than 30 major crops. Given the wide range of crops for which these preparations are offered, as well as the anti-drug strategy for the pesticides application, which involves the use of substances with a new mechanism of action and the introduction of combined formulations based on two or more active substances, it is possible to actively use pyrazolecarboxamides in one region, that is why there is a possibility of their simultaneous arrival in environmental objects.The aim ofthe study– to develop a methodology for the analytical determination of fluxapyroxad, penthiopyrad, isopyrazam and sedaxanin their joint presence in water.Materials and Methods. Chromatographic analysis was performed on liquid chromatographs LC-10ADvp and LC-20AD from Shimadzu (Japan) with ultraviolet detection.Results and Discussion. It was found that the C18 column is more promising for solving the problem of pyrazolecarboxamidesseparation under study. The gradient regime in the eluent system was recognized as optimal: A (acetonitrile), B (methanol) and C (bidistilled water). The retention time (min) is: for fluxapyroxad– 6.8±0.1; trans-sedaxan– 7.4±0.1; cis-sedaxane– 8.2±0.1; penthiopyrad– 9.3±0.1 and isopyrazam– 11.0 ± 0.1.Conclusions. The conditions for the simultaneous determination of fluxapyroxad, penthiopyrad, isopyrazam and sedaxanby the high-performance liquid chromatography method with their simultaneous presence in water sample wasdeveloped.It makes it possible to significantly accelerate the analysis and reduce the costs of conducting it.

Recent Applications of High Performance Thin Layer Chromatography and Derivative Spectrophotometry in Pharmaceutical Analysis

2020 ◽  
Vol 16 (6) ◽  
pp. 671-689
Author(s):  
Marcin Gackowski ◽  
Marcin Koba ◽  
Katarzyna Mądra-Gackowska ◽  
Piotr Kośliński ◽  
Stefan Kruszewski
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Pharmaceutical Analysis ◽  
High Performance ◽  
Degradation Products ◽  
Derivative Spectrophotometry ◽  
Accuracy And Precision ◽  
Post Marketing ◽  
Layer Chromatography

At present, no one can imagine drug development, marketing and post-marketing without rigorous quality control at each stage. Only modern, selective, accurate and precise analytical methods for determination of active compounds, their degradation products and stability studies are able to assure the appropriate amount and purity of drugs administered every day to millions of patients all over the world. For routine control of drugs simple, economic, rapid and reliable methods are desirable. The major focus of current scrutiny is placed on high-performance thin layer chromatography and derivative spectrophotometry methods, which fulfill routine drug estimation’s expectations [1-4]. The present paper reveals state-of-the-art and possible applications of those methods in pharmaceutical analysis between 2010 and 2018. The review shows advantages of high-performance thin layer chromatography and derivative spectrophotometry, including accuracy and precision comparable to more expensive and time-consuming methods as well as additional fields of possible applications, which contribute to resolving many analytical problems in everyday laboratory practice.

ICH/FDA Guidelines-Compliant Validated Stability-Indicating HPLC-UV Method for the Determination of Axitinib in Bulk and Dosage Forms

2020 ◽  
Vol 16 (8) ◽  
pp. 1106-1112
Author(s):  
Ibrahim A. Darwish ◽  
Nasr Y. Khalil ◽  
Mohammad AlZeer
Keyword(s):  
High Performance ◽  
Kinase Inhibitor ◽  
Degradation Products ◽  
Internal Standard ◽  
Dosage Forms ◽  
Uv Detector ◽  
Stability Indicating ◽  
Therapeutic Benefits ◽  
Relative Standard

Background: Axitinib (AXT) is a member of the new generation of the kinase inhibitor indicated for the treatment of advanced renal cell carcinoma. Its therapeutic benefits depend on assuring the good-quality of its dosage forms in terms of content and stability of the pharmaceutically active ingredient. Objective: This study was devoted to the development of a simple, sensitive and accurate stabilityindicating high-performance liquid chromatographic method with ultraviolet detection (HPLC-UV) for the determination of AXT in its bulk and dosage forms. Methods: Waters HPLC system was used. The chromatographic separation of AXT, internal standard (olaparib), and degradation products were performed on the Nucleosil CN column (250 × 4.6 mm, 5 μm). The mobile phase consisted of water:acetonitrile:methanol (40:40:20, v/v/v) with a flow rate of 1 ml/min, and the UV detector was set at 225 nm. AXT was subjected to different accelerated stress conditions and the degradation products, when any, were completely resolved from the intact AXT. Results: The method was linear (r = 0.9998) in the concentration range of 5-50 μg/ml. The limits of detection and quantitation were 0.85 and 2.57 μg/ml, respectively. The accuracy of the method, measured as recovery, was in the range of 98.0-103.6% with relative standard deviations in the range of 0.06-3.43%. The results of stability testing revealed that AXT was mostly stable in neutral and oxidative conditions; however, it was unstable in alkaline and acidic conditions. The kinetics of degradation were studied, and the kinetic rate constants were determined. The proposed method was successfully applied for the determination of AXT in bulk drug and dosage forms. Conclusions: A stability-indicating HPLC-UV method was developed and validated for assessing AXT stability in its bulk and dosage forms. The method met the regulatory requirements of the International Conference on Harmonization (ICH) and the Food and Drug Administration (FDA). The results demonstrated that the method would have great value when applied in quality control and stability studies for AXT.

Validated Stability Indicating HPTLC Method for the Estimation of Amoxapine in Different Stress Conditions

2019 ◽  
Vol 15 (3) ◽  
pp. 273-279
Author(s):  
Shweta G. Rangari ◽  
Nishikant A. Raut ◽  
Pradip W. Dhore
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Analysis Data ◽  
Peak Height ◽  
Good Resolution ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Wide Range ◽  
Hptlc Method

Background:The unstable and/or toxic degradation products may form due to degradation of drug which results into loss of therapeutic activity and lead to life threatening condition. Hence, it is important to establish the stability characteristics of drug in various conditions such as in temperature, light, oxidising agent and susceptibility across a wide range of pH values.Introduction:The aim of the proposed study was to develop simple, sensitive and economic stability indicating high performance thin layer chromatography (HPTLC) method for the quantification of Amoxapine in the presence of degradation products.Methods:Amoxapine and its degraded products were separated on precoated silica gel 60F254 TLC plates by using mobile phase comprising of methanol: toluene: ammonium acetate (6:3:1, v/v/v). The densitometric evaluation was carried out at 320 nm in reflectance/absorbance mode. The degradation products obtained as per ICH guidelines under acidic, basic and oxidative conditions have different Rf values 0.12, 0.26 and 0.6 indicating good resolution from each other and pure drug with Rf: 0.47. Amoxapine was found to be stable under neutral, thermal and photo conditions.Results:The method was validated as per ICH Q2 (R1) guidelines in terms of accuracy, precision, ruggedness, robustness and linearity. A good linear relationship between concentration and response (peak area and peak height) over the range of 80 ng/spot to 720 ng/spot was observed from regression analysis data showing correlation coefficient 0.991 and 0.994 for area and height, respectively. The limit of detection (LOD) and limit of quantitation (LOQ) for area were found to be 1.176 ng/mL and 3.565 ng/mL, whereas for height, 50.063 ng/mL and 151.707 ng/mL respectively.Conclusion:The statistical analysis confirmed the accuracy, precision and selectivity of the proposed method which can be effectively used for the analysis of amoxapine in the presence of degradation products.

scholarly journals Applicability of Cork as Novel Modifiers to Develop Electrochemical Sensor for Caffeine Determination

Materials ◽  
2020 ◽  
Vol 14 (1) ◽  
pp. 37
Author(s):  
Mayra K. S. Monteiro ◽  
Djalma R. Da Silva ◽  
Marco A. Quiroz ◽  
Vítor J. P. Vilar ◽  
Carlos A. Martínez-Huitle ◽  
...  
Keyword(s):  
Electrochemical Sensor ◽  
Linear Response ◽  
High Performance ◽  
Low Cost ◽  
Pharmaceutical Formulations ◽  
Caffeine Concentration ◽  
Real Samples ◽  
Wide Range ◽  
Potential Use

This study aims to investigate the applicability of a hybrid electrochemical sensor composed of cork and graphite (Gr) for detecting caffeine in aqueous solutions. Raw cork (RAC) and regranulated cork (RGC, obtained by thermal treatment of RAC with steam at 380 °C) were tested as modifiers. The results clearly showed that the cork-graphite sensors, GrRAC and GrRGC, exhibited a linear response over a wide range of caffeine concentration (5–1000 µM), with R2 of 0.99 and 0.98, respectively. The limits of detection (LOD), estimated at 2.9 and 6.1 µM for GrRAC and GrRGC, suggest greater sensitivity and reproducibility than the unmodified conventional graphite sensor. The low-cost cork-graphite sensors were successfully applied in the determination of caffeine in soft drinks and pharmaceutical formulations, presenting well-defined current signals when analyzing real samples. When comparing electrochemical determinations and high performance liquid chromatography measurements, no significant differences were observed (mean accuracy 3.0%), highlighting the potential use of these sensors to determine caffeine in different samples.

scholarly journals Strength Analysis of Alternative Airframe Layouts of Regional Aircraft on the Basis of Automated Parametrical Models

Aerospace ◽  
2021 ◽  
Vol 8 (3) ◽  
pp. 80
Author(s):  
Dmitry V. Vedernikov ◽  
Alexander N. Shanygin ◽  
Yury S. Mirgorodsky ◽  
Mikhail D. Levchenkov
Keyword(s):  
Aspect Ratio ◽  
High Aspect Ratio ◽  
High Performance ◽  
Strength Analysis ◽  
Labor Input ◽  
Aerodynamic Loading ◽  
Aspect Ratios ◽  
Wide Range ◽  
Parametrical Design

This publication presents the results of complex parametrical strength investigations of typical wings for regional aircrafts obtained by means of the new version of the four-level algorithm (FLA) with the modified module responsible for the analysis of aerodynamic loading. This version of FLA, as well as a base one, is focused on significant decreasing time and labor input of a complex strength analysis of airframes by using simultaneously different principles of decomposition. The base version includes four-level decomposition of airframe and decomposition of strength tasks. The new one realizes additional decomposition of alternative variants of load cases during the process of determination of critical load cases. Such an algorithm is very suitable for strength analysis and designing airframes of regional aircrafts having a wide range of aerodynamic concepts. Results of validation of the new version of FLA for a high-aspect-ratio wing obtained in this work confirmed high performance of the algorithm in decreasing time and labor input of strength analysis of airframes at the preliminary stages of designing. During parametrical design investigation, some interesting results for strut-braced wings having high aspect ratios were obtained.

scholarly journals Determination of amino acids in human biological fluids by high-performance liquid chromatography: critical review

Amino Acids ◽  
2021 ◽  
Author(s):  
Grażyna Gałęzowska ◽  
Joanna Ratajczyk ◽  
Lidia Wolska
Keyword(s):  
Amino Acids ◽  
Amino Acid ◽  
High Performance ◽  
Hplc Analysis ◽  
Limit Of Detection ◽  
Biological Fluids ◽  
Analytical Techniques ◽  
Epidemiological Studies ◽  
Preparation Conditions

AbstractThe quantitation and qualification of amino acids are most commonly used in clinical and epidemiological studies, and provide an excellent way of monitoring compounds in human fluids which have not been monitored previously, to prevent some diseases. Because of this, it is not surprising that scientific interest in evaluating these compounds has resurfaced in recent years and has precipitated the development of a multitude of new analytical techniques. This review considers recent developments in HPLC analytics on the basis of publications from the last few years. It helps to update and systematize knowledge in this area. Particular attention is paid to the progress of analytical methods, pointing out the advantages and drawbacks of the various techniques used for the preparation, separation and determination of amino acids. Depending on the type of sample, the preparation conditions for HPLC analysis change. For this reason, the review has focused on three types of samples, namely urine, blood and cerebrospinal fluid. Despite time-consuming sample preparation before HPLC analysis, an additional derivatization technique should be used, depending on the detection technique used. There are proposals for columns that are specially modified for amino acid separation without derivatization, but the limit of detection of the substance is less beneficial. In view of the fact that amino acid analyses have been performed for years and new solutions may generate increased costs, it may turn out that older proposals are much more advantageous.

scholarly journals A Selective High-Performance Liquid Chromatography Method for the Determination of Reboxetine in Bulk Drug and Tablets

2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Depressive Disorders ◽  
Degradation Products ◽  
Severe Depression ◽  
Hplc Method ◽  
Chromatography Method ◽  
Relative Standard

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.

Development and validation of a fast and simple HPLC method for the simultaneous determination of aniline and its degradation products in wastewater

2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Simple Method ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Development And Validation

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.

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