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papers from the latest issue:
The paradigm shifting role of chromatographic methods in pharmaceutical analysis
22 August 2012,
08:25:36
Publication year:
2012
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
Sándor Görög
An overview is presented of the impact of chromatographic method developments on the quality control of pharmaceuticals as of the 1950s up until the present times. This survey is mainly based on the changes in pharmacopeias starting with United States Pharmacopeia (USP) 16, issued in 1960, up to the presently effective USP 34 and European Pharmacopeia 7.2. At the beginning of this period the role of chromatographic methods was negligible and was restricted to classical column chromatography and paper chromatography. However, the invention of high-performance liquid chromatography (HPLC) initiated a rapid paradigm shift in the attitude toward, and the use of, chromatographic methods. As a result, HPLC began a “career” of rapid spreading and development, and by now has undoubtedly become the principal method in pharmaceutical analysis. Likewise, the role of thin-layer chromatography (TLC) and to a lesser extent gas chromatography is also remarkable. The role of these and electrophoretic methods in the identification, assay and purity check of drugs and drug products in the modern pharmacopeias is discussed. As a case study the stability investigation of Depersolone® injection carried out in the 1960s and 35 years later is presented and the information obtainable from the classical and modern approach is compared.
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
Sándor Görög
An overview is presented of the impact of chromatographic method developments on the quality control of pharmaceuticals as of the 1950s up until the present times. This survey is mainly based on the changes in pharmacopeias starting with United States Pharmacopeia (USP) 16, issued in 1960, up to the presently effective USP 34 and European Pharmacopeia 7.2. At the beginning of this period the role of chromatographic methods was negligible and was restricted to classical column chromatography and paper chromatography. However, the invention of high-performance liquid chromatography (HPLC) initiated a rapid paradigm shift in the attitude toward, and the use of, chromatographic methods. As a result, HPLC began a “career” of rapid spreading and development, and by now has undoubtedly become the principal method in pharmaceutical analysis. Likewise, the role of thin-layer chromatography (TLC) and to a lesser extent gas chromatography is also remarkable. The role of these and electrophoretic methods in the identification, assay and purity check of drugs and drug products in the modern pharmacopeias is discussed. As a case study the stability investigation of Depersolone® injection carried out in the 1960s and 35 years later is presented and the information obtainable from the classical and modern approach is compared.
New trends in reversed-phase liquid chromatographic separations of therapeutic peptides and proteins: Theory and applications
22 August 2012,
08:25:36
Publication year:
2012
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
Szabolcs Fekete, Jean-Luc Veuthey, Davy Guillarme
In the pharmaceutical field, there is considerable interest in the use of peptides and proteins for therapeutic purposes. There are various ways to characterize such complex samples, but during the last few years, a significant number of technological developments have been brought to the field of RPLC and RPLC–MS. Thus, the present review focuses first on the basics of RPLC for peptides and proteins, including the inherent problems, some possible solutions and some directions for developing a new RPLC method that is dedicated to biomolecules. Then the latest advances in RPLC, such as wide-pore core–shell particles, fully porous sub-2μm particles, organic monoliths, porous layer open tubular columns and elevated temperature, are described and critically discussed in terms of both kinetic efficiency and selectivity. Numerous applications with real samples are presented that confirm the relevance of these different strategies. Finally, one of the key advantages of RPLC for peptides and proteins over other historical approaches is its inherent compatibility with MS using both MALDI and ESI sources.
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
Szabolcs Fekete, Jean-Luc Veuthey, Davy Guillarme
In the pharmaceutical field, there is considerable interest in the use of peptides and proteins for therapeutic purposes. There are various ways to characterize such complex samples, but during the last few years, a significant number of technological developments have been brought to the field of RPLC and RPLC–MS. Thus, the present review focuses first on the basics of RPLC for peptides and proteins, including the inherent problems, some possible solutions and some directions for developing a new RPLC method that is dedicated to biomolecules. Then the latest advances in RPLC, such as wide-pore core–shell particles, fully porous sub-2μm particles, organic monoliths, porous layer open tubular columns and elevated temperature, are described and critically discussed in terms of both kinetic efficiency and selectivity. Numerous applications with real samples are presented that confirm the relevance of these different strategies. Finally, one of the key advantages of RPLC for peptides and proteins over other historical approaches is its inherent compatibility with MS using both MALDI and ESI sources.
Highlights
► RPLC is a powerful strategy for peptide and protein separations. ► The new wide-pore UHPLC and core–shell particles provide some impressive results even with large proteins. ► Elevated mobile phase temperature is an additional parameter for improving separations of large biomolecules. ► Trends in RPLC method development of proteins and peptides are presented. ► The most important advantage of RPLC over IEX is its inherent compatibility with ESI-MS.Recent advances in the direct and indirect liquid chromatographic enantioseparation of amino acids and related compounds: A review
22 August 2012,
08:25:36
Publication year:
2012
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
István Ilisz, Anita Aranyi, Zoltán Pataj, Antal Péter
Amino acids are essential for life, and have many functions in metabolism. One particularly important function is to serve as the building blocks of peptides and proteins, giving rise to complex three dimensional structures through disulfide bonds or crosslinked amino acids. Peptides are frequently cyclic and contain protein as well as non-protein aminoacids in many instances. Since most of the proteinogenic α-amino acids contain a chiral carbon atom (with the exception of glycine), the stereoisomers of all these amino acids and the peptides in which they are to be found may possess differences in biological activity in living systems. The impetus for advances in chiral separation has been highest in the past decade and this still continues to be an area of high focus. The important analytical task of the separation of isomers is achieved mainly by chromatographic methods. This review surveys indirect and direct HPLC separations of biologically and pharmaceutically important enantiomers of amino acids and related compounds, with emphasis on the literature published from 2005.
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
István Ilisz, Anita Aranyi, Zoltán Pataj, Antal Péter
Amino acids are essential for life, and have many functions in metabolism. One particularly important function is to serve as the building blocks of peptides and proteins, giving rise to complex three dimensional structures through disulfide bonds or crosslinked amino acids. Peptides are frequently cyclic and contain protein as well as non-protein aminoacids in many instances. Since most of the proteinogenic α-amino acids contain a chiral carbon atom (with the exception of glycine), the stereoisomers of all these amino acids and the peptides in which they are to be found may possess differences in biological activity in living systems. The impetus for advances in chiral separation has been highest in the past decade and this still continues to be an area of high focus. The important analytical task of the separation of isomers is achieved mainly by chromatographic methods. This review surveys indirect and direct HPLC separations of biologically and pharmaceutically important enantiomers of amino acids and related compounds, with emphasis on the literature published from 2005.
Highlights
► Chiral separation of amino acid enantiomers applying chiral derivatizing agents (CDAs). ► Application of chiral stationary phases (CSPs) in the enantioseparation of amino acids. ► Application of cyclodextrin- and macrocyclic glycopeptide based CSPs. ► Application of chiral crown ether-, quninine-, and polysaccharide-based CSPs.HPLC analysis of naturally occurring free d-amino acids in mammals
22 August 2012,
08:25:36
Publication year:
2012
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
Yurika Miyoshi, Reiko Koga, Tsubasa Oyama, Hai Han, Kyoko Ueno, Kei Masuyama, Yusuke Itoh, Kenji Hamase
d-Amino acids are currently recognized as naturally occurring physiologically active substances and biomarkers in mammals. The progress of analytical technologies, mostly high resolution chromatographic or electrodriven separation methods, has significantly contributed to the advances in d-amino acid research in real biological matrices. In this review, we would like to describe the d-amino acid research, from the discovery of appreciable amounts of free d-amino acids in mammals to the current metabolomics study focusing on amino acid enantiomers. The liquid phase enantioselective analytical methods utilized for the determination of d-amino acids in mammals including human beings will be discussed.
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
Yurika Miyoshi, Reiko Koga, Tsubasa Oyama, Hai Han, Kyoko Ueno, Kei Masuyama, Yusuke Itoh, Kenji Hamase
d-Amino acids are currently recognized as naturally occurring physiologically active substances and biomarkers in mammals. The progress of analytical technologies, mostly high resolution chromatographic or electrodriven separation methods, has significantly contributed to the advances in d-amino acid research in real biological matrices. In this review, we would like to describe the d-amino acid research, from the discovery of appreciable amounts of free d-amino acids in mammals to the current metabolomics study focusing on amino acid enantiomers. The liquid phase enantioselective analytical methods utilized for the determination of d-amino acids in mammals including human beings will be discussed.
Charged aerosol detection in pharmaceutical analysis
22 August 2012,
08:25:36
Publication year:
2012
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
Stefan Almeling, David Ilko, Ulrike Holzgrabe
Due to its wide field of application, sensitivity, wide range of linearity and the applicability to gradient elution, the most common detection technique for HPLC nowadays is UV/vis spectrophotometry. However, UV/vis detection comes to its limits when the analytes are lacking suitable chromophors or exhibit very different UV responses. In the past years, different types of evaporation/aerosol based HPLC detectors have been developed to fill this gap in HPLC detection. Amongst those, the corona-charged aerosol detector (CAD) is one of the most powerful and versatile representatives. In the recent past a variety of papers have been published, demonstrating the potential of the CAD in different fields of analytical chemistry. This paper is intended to provide an overview of the key performance characteristics and manifold applications for HPLC-CAD in the field of pharmaceutical analysis.
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
Stefan Almeling, David Ilko, Ulrike Holzgrabe
Due to its wide field of application, sensitivity, wide range of linearity and the applicability to gradient elution, the most common detection technique for HPLC nowadays is UV/vis spectrophotometry. However, UV/vis detection comes to its limits when the analytes are lacking suitable chromophors or exhibit very different UV responses. In the past years, different types of evaporation/aerosol based HPLC detectors have been developed to fill this gap in HPLC detection. Amongst those, the corona-charged aerosol detector (CAD) is one of the most powerful and versatile representatives. In the recent past a variety of papers have been published, demonstrating the potential of the CAD in different fields of analytical chemistry. This paper is intended to provide an overview of the key performance characteristics and manifold applications for HPLC-CAD in the field of pharmaceutical analysis.
New monolithic chromatographic supports for macromolecules immobilization: Challenges and opportunities
22 August 2012,
08:25:36
Publication year:
2012
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
E. Calleri, S. Ambrosini, C. Temporini, G. Massolini
This mini-review reports on some recent advances in the field of immobilized protein employing both silica and polymer-based monoliths as supports, and their application in affinity chromatography and immobilized enzyme reactors (IMERs) developments. The major emphasis is put on some interesting challenges and opportunities related to the development of new monolithic affinity supports based on biofriendly sol–gel inorganic monoliths with entrapped proteins and on organic monolithic supports with improved hydrophilicity for IMERs development in proteomic studies. The ease of preparation of monoliths and the multitude of functionalization techniques, make monoliths interesting for an increasing number of biochemical and medical applications.
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
E. Calleri, S. Ambrosini, C. Temporini, G. Massolini
This mini-review reports on some recent advances in the field of immobilized protein employing both silica and polymer-based monoliths as supports, and their application in affinity chromatography and immobilized enzyme reactors (IMERs) developments. The major emphasis is put on some interesting challenges and opportunities related to the development of new monolithic affinity supports based on biofriendly sol–gel inorganic monoliths with entrapped proteins and on organic monolithic supports with improved hydrophilicity for IMERs development in proteomic studies. The ease of preparation of monoliths and the multitude of functionalization techniques, make monoliths interesting for an increasing number of biochemical and medical applications.
Supercritical fluid chromatography for the enantioseparation of pharmaceuticals
22 August 2012,
08:25:36
Publication year:
2012
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
Katrijn De Klerck, Debby Mangelings, Yvan Vander Heyden
Chirality has a significant impact on drug discovery and development processes in the pharmaceutical industry. As the number of enantiopure drugs launched onto the market is yearly increasing, the need for fast and performant enantioseparation methods with minimal costs is becoming more compelling. In this context, sub- and supercritical fluid chromatography (SFC), being applicable at an analytical, as well as at a preparative scale is gaining more interest. In this review a practical overview is given of the different parameters that are important in supercritical fluid chromatographic separations. A comparison is made between the applicability for chiral separations of SFC and conventional high-performance liquid chromatography (HPLC), and illustrated by means of examples. Different aspects of method development and the upscaling feasibility in SFC are discussed. This review aims to give the reader a practical insight in the use of supercritical fluid chromatography for the chiral separation of pharmaceutical compounds.
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
Katrijn De Klerck, Debby Mangelings, Yvan Vander Heyden
Chirality has a significant impact on drug discovery and development processes in the pharmaceutical industry. As the number of enantiopure drugs launched onto the market is yearly increasing, the need for fast and performant enantioseparation methods with minimal costs is becoming more compelling. In this context, sub- and supercritical fluid chromatography (SFC), being applicable at an analytical, as well as at a preparative scale is gaining more interest. In this review a practical overview is given of the different parameters that are important in supercritical fluid chromatographic separations. A comparison is made between the applicability for chiral separations of SFC and conventional high-performance liquid chromatography (HPLC), and illustrated by means of examples. Different aspects of method development and the upscaling feasibility in SFC are discussed. This review aims to give the reader a practical insight in the use of supercritical fluid chromatography for the chiral separation of pharmaceutical compounds.
Highlights
► A practical overview of different parameters that are important for the chiral separation of pharmaceuticals with SFC. ► Comparison of chiral SFC and HPLC, illustrated with examples. ► Method development aspects and upscaling feasibility in SFC. ► New developments in the field of SFC.Pharmaceutical and biomedical applications of affinity chromatography: Recent trends and developments
22 August 2012,
08:25:36
Publication year:
2012
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
David S. Hage, Jeanethe A. Anguizola, Cong Bi, Rong Li, Ryan Matsuda, Efthimia Papastavros, Erika Pfaunmiller, John Vargas, Xiwei Zheng
Affinity chromatography is a separation technique that has become increasingly important in work with biological samples and pharmaceutical agents. This method is based on the use of a biologically related agent as a stationary phase to selectively retain analytes or to study biological interactions. This review discusses the basic principles behind affinity chromatography and examines recent developments that have occurred in the use of this method for biomedical and pharmaceutical analysis. Techniques based on traditional affinity supports are discussed, but an emphasis is placed on methods in which affinity columns are used as part of HPLC systems or in combination with other analytical methods. General formats for affinity chromatography that are considered include step elution schemes, weak affinity chromatography, affinity extraction and affinity depletion. Specific separation techniques that are examined include lectin affinity chromatography, boronate affinity chromatography, immunoaffinity chromatography, and immobilized metal ion affinity chromatography. Approaches for the study of biological interactions by affinity chromatography are also presented, such as the measurement of equilibrium constants, rate constants, or competition and displacement effects. In addition, related developments in the use of immobilized enzyme reactors, molecularly imprinted polymers, dye ligands and aptamers are briefly considered.
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
David S. Hage, Jeanethe A. Anguizola, Cong Bi, Rong Li, Ryan Matsuda, Efthimia Papastavros, Erika Pfaunmiller, John Vargas, Xiwei Zheng
Affinity chromatography is a separation technique that has become increasingly important in work with biological samples and pharmaceutical agents. This method is based on the use of a biologically related agent as a stationary phase to selectively retain analytes or to study biological interactions. This review discusses the basic principles behind affinity chromatography and examines recent developments that have occurred in the use of this method for biomedical and pharmaceutical analysis. Techniques based on traditional affinity supports are discussed, but an emphasis is placed on methods in which affinity columns are used as part of HPLC systems or in combination with other analytical methods. General formats for affinity chromatography that are considered include step elution schemes, weak affinity chromatography, affinity extraction and affinity depletion. Specific separation techniques that are examined include lectin affinity chromatography, boronate affinity chromatography, immunoaffinity chromatography, and immobilized metal ion affinity chromatography. Approaches for the study of biological interactions by affinity chromatography are also presented, such as the measurement of equilibrium constants, rate constants, or competition and displacement effects. In addition, related developments in the use of immobilized enzyme reactors, molecularly imprinted polymers, dye ligands and aptamers are briefly considered.
Structure elucidation of indole–indoline type alkaloids: A retrospective account from the point of view of current NMR and MS technology
22 August 2012,
08:25:36
Publication year:
2012
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
Zoltán Béni, Viktor Háda, Zsófia Dubrovay, Csaba Szántay
In this review our aim is to look back on how the structure elucidation of bisindoles, especially with focus placed on vinblastine and vincristine analogues, has evolved alongside with the development of MS and NMR over the last 60 years from the perspective of our present-day use of state-of-the-art MS and NMR instrumentation and on the basis of our own accumulated views and experience in the field.
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
Zoltán Béni, Viktor Háda, Zsófia Dubrovay, Csaba Szántay
In this review our aim is to look back on how the structure elucidation of bisindoles, especially with focus placed on vinblastine and vincristine analogues, has evolved alongside with the development of MS and NMR over the last 60 years from the perspective of our present-day use of state-of-the-art MS and NMR instrumentation and on the basis of our own accumulated views and experience in the field.
Highlights
► The challenges of determining the structure of bisindoles. ► Historical roles of NMR and mass spectrometry in bisindole structure elucidation. ► The capabilities of modern NMR and MS in bisindole structure elucidation. ► Demonstrative examples are discussed for vinblastine and vincristine analogues.Critical review of near-infrared spectroscopic methods validations in pharmaceutical applications
22 August 2012,
08:25:36
Publication year:
2012
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
C. De Bleye, P.-F. Chavez, J. Mantanus, R. Marini, Ph. Hubert, E. Rozet, E. Ziemons
Based on the large number of publications reported over the past five years, near-infrared spectroscopy (NIRS) is more and more considered an attractive and promising analytical tool regarding Process Analytical Technology and Green Chemistry. From the reviewed literature, few of these publications present a thoroughly validated NIRS method even if some guidelines have been published by different groups and regulatory authorities. However, as any analytical method, the validation of NIRS method is a mandatory step at the end of the development in order to give enough guarantees that each of the future results during routine use will be close enough to the true value. Besides the introduction of PAT concepts in the revised document of the European Pharmacopoeia (2.2.40) dealing with near-infrared spectroscopy recently published in Pharmeuropa, it agrees very well with this mandatory step. Indeed, the latter suggests to use similar analytical performance characteristics than those required for any analytical procedure based on acceptance criteria consistent with the intended use of the method. In this context, this review gives a comprehensive and critical overview of the methodologies applied to assess the validity of quantitative NIRS methods used in pharmaceutical applications.
Source:Journal of Pharmaceutical and Biomedical Analysis, Volume 69
C. De Bleye, P.-F. Chavez, J. Mantanus, R. Marini, Ph. Hubert, E. Rozet, E. Ziemons
Based on the large number of publications reported over the past five years, near-infrared spectroscopy (NIRS) is more and more considered an attractive and promising analytical tool regarding Process Analytical Technology and Green Chemistry. From the reviewed literature, few of these publications present a thoroughly validated NIRS method even if some guidelines have been published by different groups and regulatory authorities. However, as any analytical method, the validation of NIRS method is a mandatory step at the end of the development in order to give enough guarantees that each of the future results during routine use will be close enough to the true value. Besides the introduction of PAT concepts in the revised document of the European Pharmacopoeia (2.2.40) dealing with near-infrared spectroscopy recently published in Pharmeuropa, it agrees very well with this mandatory step. Indeed, the latter suggests to use similar analytical performance characteristics than those required for any analytical procedure based on acceptance criteria consistent with the intended use of the method. In this context, this review gives a comprehensive and critical overview of the methodologies applied to assess the validity of quantitative NIRS methods used in pharmaceutical applications.
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