Analytical Chemistry Principles Research Articles

Efficient integration of analytical quality-by-design and tri-hued HPLC-DAD approach for synchronized assessment of gemigliptin and rosuvastatin in their fixed-dose pills: Application to stability study

Life-threatening atherosclerotic cardiovascular disorder is a well-recognized risk among diabetics, which is clinically ascribed to their unbalanced plasma lipoproteins. Gemigliptin-Rosuvastatin is a recently introduced polytherapy prescribed for the management of diabetic dyslipidemia. Currently, the main focus of several analysts is to design more ecologically friendly sustainable approaches for pharmaceutical analysis. In this context, an innovative tri-hued (green, blue, and white) stability-indicating HPLC-DAD approach was developed to concurrently quantify Gemigliptin and Rosuvastatin polypills. Consequently, a strategic integration between analytical quality-by-design and green/white analytical chemistry principles was specifically designed to optimize efficiency and practicality while minimizing ecological burden. Two experimental designs, namely two-level fractional factorial and Box-Behnken designs, were employed for screening and optimization procedures, respectively. Optimal separation was attained utilizing an Agilent HC-C18 column in conjunction with a mobile phase consisting of acetonitrile and 10 mM sodium dihydrogen phosphate buffer, pH 3 (60:40 v/v), eluted in an isocratic manner at a 1 mL/min flow rate. Both analytes exhibited good linearities within the concentration range of 0.5–100 μg/mL. Furthermore, stability studies were conducted on both drugs in response to variable stress degradation scenarios. Fortunately, the adopted approach was well-suited to resolve the studied drugs from their respective degradants, thereby verifying the method's stability-indicating power. Tri-hued evaluation for the implemented approach was performed via up-to-date metrics, specifically, the Analytical Eco-scale, AGREE, Blue Applicability Grade Index, and RGB 12. Ultimately, our adopted stability-indicating HPLC approach exhibited great sensitivity, specificity, applicability, and rapidity as well as being ecologically sound. It is worth noting that this is the first stability-indicating HPLC approach for simultaneous assessment of the studied drugs.

BrJAC mourns the death of Prof. Dr. Miguel Valcárcel Cases and recognizes his great contribution to Analytical Chemistry and Science around the World

Who has not seen or heard about books such as Analytical Chemistry: A Modern Approach to Analytical Science, Principles of Analytical Chemistry: A Textbook, or Foundations of Analytical Chemistry: A Teaching-Learning Approach, or about flow injection analysis-FIA, and sequential injection analysis-SIA? These are, in fact, some contributions from Prof. Miguel Valcárcel Cases, at the University of Córdoba-Spain, who leave us on 9th January 2022 at the age of 75. Prof. Valcárcel was Dean of the Faculty of Sciences at the University of Córdoba, Vice-Rector for academic guidance and teaching and Vice-Rector for quality, as well as the first Director of the Andalusian Institute of Fine Chemistry and Nanochemistry since 1994. Born in Barcelona (Spain), Prof. Valcárcel was a graduate of the University of Seville where also obtained his Ph.D., and was an assistant teacher until 1975. He was an associate professor of Analytical Chemistry at the Faculty of Science of Palma de Mallorca in 1975, an institution where he was also Dean and full professor at the University of Cordoba in the year 1976. He was also President of the Analytical Division of the European Federation of Chemical Societies and was a member for 4 years of the High-Level Expert Group of the European Union's Growth Program. Valcárcel received the Spanish national Enrique Moles prize for Chemical Science and Technology (2005), the Maimónides prize for scientific-technical research from the Junta de Andalucia (1992), and the Solvay Research Prize in Chemical Sciences from the CEOE Foundation (1997). He has the Robert Boyle Medal from the Royal Society of Chemistry (UK, 2004), the Enrich Planquette Prize from the Austrian Chemical Society (1996), the Gold Medal from the University of Warsaw (2000), and the Medal from the Portuguese Chemical Society (2000). He also received the distinction of Cordoba citizen of the year 2006 in the education/research section, and the Averroes de Oro-Cuidad de Córdoba medal in 2006 for his scientific trajectory. He was also awarded the title of Doctor Honoris Causa by the University of Valencia (2010) and the European DAC-EuChMS (Division of Analytical Chemistry of the European Association for Chemical and Molecular Sciences) award in recognition of his scientific and teaching career (2015). He was the author of ca. 700 papers, published 9 scientific books, and co-authored 15 chapters of multi-author books. Owner of a unique vitality and a very accurate vision of Analytical Chemistry, Prof. Valcárcel contributed to the formation of dozens of students, of which he was extremely proud, and some of them are today Full professors spread all over the world. The Brazilian Journal of Analytical Chemistry mourns his death, and through this simple tribute, recognizes his great contribution to Analytical Chemistry and science around the world.

Lipid Metabolism and Lipidomics Applications in Cancer Research.

Lipids are the critical components of cellular and plasma membrane, which constitute an impermeable barrier of cellular compartments, and play important roles on numerous cellular processes including cell growth, proliferation, differentiation, and signaling. Alterations in lipid metabolism have been implicated in the development and progression of cancers. However, unlike other biomolecules, the diversity in the structures and characteristics of lipid species results in the limited understanding of their metabolic alterations in cancers. Lipidomics is an emerging discipline that studies lipids in a large scale based on analytical chemistry principles and technological tools. Multidimensional mass spectrometry-based shotgun lipidomics (MDMS-SL) uses direct infusion to avoid difficulties from alterations in concentration, chromatographic anomalies, and ion-pairing alterations to improve resolution and achieve rapid and accurate qualitative and quantitative analysis. In this chapter, lipids and lipid metabolism relevant to cancer research are introduced, followed by a brief description of MDMS-SL and other shotgun lipidomics techniques and some applications for cancer research.

Use of eosin for green spectroscopic determination of mebendazole.

New, sensitive, and reliable spectroscopic methods were constructed for the fast determination of the anthelmintic drug mebendazole. The methods depended on the reaction of the amino group in mebendazole with eosin in acidic medium forming an ion pair complex. The first method, Method I, relied on quenching of the native fluorescence of eosin after reaction with mebendazole at pH 3.7 using acetate buffer. Fluorescence quenching was measured at 538 nm after excitation at 518 nm. This method showed a linear response over the concentration range 5.0-20.0 μg/ml. The second method, Method II, was based on measuring the absorbance of the formed complex at 554 nm; the method showed good linearity from 7.0 to 22.0 μg/ml. Different parameters that influenced the formation of the reaction product were carefully investigated to reach the optimized conditions. A comparison between the proposed methods and a previous spectrophotometric method was carried out and there was no significant difference between them. The methods could be applied successfully to determine mebendazole in its tablet form. Moreover, the methods used water as diluting solvent, which made them compatible with the 'green' analytical chemistry principles. No organic solvents were used throughout the study.

Green Analytical Chemistry, Opportunities for Pharmaceutical Quality Control

This review article summarizes the opportunities for utilizing the green analytical chemistry (GAC) techniques and principles in the field of quality control (Q.C) of the pharmaceuticals. Green analytical chemistry is considered a branch of the green chemistry which is based on principles overlap with the sustained development ultimate goals. General definitions of quality and quality control, principles of Green Analytical Chemistry, proposals for greener sample pre-treatment, and greener chromatographic method of analysis to be applied in QC laboratories are herein discussed. The main goal is achieving more eco- friendly analysis in QC laboratories through different strategies and techniques replace the toxic reagents, and to modify or replace analytical methods and/or techniques with safer ones, making it possible to dramatically reduce the amounts of reagents consumed and waste generated. General definitions for quality and quality control: There are Several definitions of the term “quality”, yet one of them is of top importance to the perception of “Managing for Quality” concept. This definition describes product quality as “those features of products which meet customer needs and the freedom from deficiencies hereby provide customer satisfaction”. Managing for quality makes extensive use of three managerial processes: 1- Quality planning; 2- Quality control; 3- Quality improvement.

Lipidomics for studying metabolism.

Many thousands of lipid species exist and their metabolism is interwoven via numerous pathways and networks. These networks can also change in response to cellular environment alterations, such as exercise or development of a disease. Measuring such alterations and understanding the pathways involved is crucial to fully understand cellular metabolism. Such demands have catalysed the emergence of lipidomics, which enables the large-scale study of lipids using the principles of analytical chemistry. Mass spectrometry, largely due to its analytical power and rapid development of new instruments and techniques, has been widely used in lipidomics and greatly accelerated advances in the field. This Review provides an introduction to lipidomics and describes some common, but important, cellular metabolic networks that can aid our understanding of metabolic pathways. Some representative applications of lipidomics for studying lipid metabolism and metabolic diseases are highlighted, as well as future applications for the use of lipidomics in studying metabolic pathways.

Protein Quantification by Elemental Mass Spectrometry: An Experiment for Graduate Students

A multiday laboratory experiment was designed to integrate inductively coupled plasma–mass spectrometry (ICP–MS) in the context of protein quantification into an advanced practical course in analytical and environmental chemistry. Graduate students were familiar with the analytical methods employed, whereas the combination of bioanalytical assays with ICP–MS is rare. Small groups of graduate students quantified ovalbumin in hen egg white using metal-coded affinity tagging (MeCAT). Proteins were covalently labeled with lanthanide chelate complexes and quantified according to the lanthanide content by ICP–MS using internal and external standards. The results were in good agreement with reference values. As an alternative approach, a Bradford assay was used for determination of the ovalbumin content of the internal standard. The chosen workflow provides hands-on experiences for the students in principles of analytical chemistry, quantitative protein analyses, gel electrophoresis, ICP–MS, calibration, and dat...

Book Review: Principles of Analytical Chemistry. A Textbook. By Miguel Valcárcel

Book Review: Principles of Analytical Chemistry. A Textbook. By Miguel Valcárcel

Quality analysis of USGS precipitation chemistry data for New York

A quality analysis of the USGS precipitation chemistry data set for New York was conducted based on analytical chemistry principles. Results indicate that the primary pattern in the data is explained by reported hydrogen ion concentrations, as measured by pH, being too high for several samples. These samples are strongly associated with low pH values reported for the later collection years, particularly 1975–1977. No meaningful pH or ion concentration trend analysis is possible with the USGS data until these suspect data points have been resolved.

Book Review: Grundlagen der analytischen Chemie. Unter besonderer Berücksichtigung der Chemie in wäßrigen Systemen. (Principles of Analytical Chemistry. With Special Reference to Chemistry in Aqueous Systems). By F. Seel

Angewandte Chemie International Edition in EnglishVolume 16, Issue 2 p. 123-123 Book Review Book Review: Grundlagen der analytischen Chemie. Unter besonderer Berücksichtigung der Chemie in wäßrigen Systemen. (Principles of Analytical Chemistry. With Special Reference to Chemistry in Aqueous Systems). By F. Seel Robert Kellner, Robert KellnerSearch for more papers by this author Robert Kellner, Robert KellnerSearch for more papers by this author First published: February 1977 https://doi.org/10.1002/anie.197701231AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinked InRedditWechat No abstract is available for this article. Volume16, Issue2February 1977Pages 123-123 RelatedInformation

Book Review: Grundlagen der analytischen Chemie (Principles of Analytical Chemistry). By F. Seel

Angewandte Chemie International Edition in EnglishVolume 9, Issue 12 p. 968-968 Book Review Book Review: Grundlagen der analytischen Chemie (Principles of Analytical Chemistry). By F. Seel Gerhard Geier, Gerhard GeierSearch for more papers by this author Gerhard Geier, Gerhard GeierSearch for more papers by this author First published: December 1970 https://doi.org/10.1002/anie.197009681AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinked InRedditWechat No abstract is available for this article. Volume9, Issue12December 1970Pages 968-968 RelatedInformation

Principles of Analytical Inorganic Chemistry

Grundlagen der analytischen Chemie und der Chemie in wasserigen Systemen Von Prof. F. Seel. Pp. 348. (Weinheim/Bergstr.: Verlag Chemie, 1955.) 29 D. marks.