LC*GC

August 2018
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COLUMNS

• SAMPLE PREP PERSPECTIVES
  The Vital Role of Blanks in Sample Preparation
  Douglas E. Raynie
  Blanks are important in the pursuits of quality control and robust quantitative analytical methods, but many analysts don’t fully understand their value, or how to use them correctly.
  
• LC TROUBLESHOOTING
  Contaminants Everywhere! Tips and Tricks for Reducing Background Signals When Using LC–MS
  Dwight R. Stoll
  We examine instances where contaminants are problematic in LC–MS, as well as successful methods to decrease their influence.
  
• PERSPECTIVES IN MODERN HPLC
  Ten Common-Sense Corollaries in Pharmaceutical Analysis by HPLC
  Michael W. Dong
  These ten propositions are widely acknowledged, but frequently neglected, by practitioners of high performance liquid chromatography (HPLC).
  
• THE ESSENTIALS
  Advantages of Supported Liquid Extraction
  We look at a process that can overcome the shortcomings associated with liquid–liquid extraction.
  

PEER-REVIEWED ARTICLES

• Frontiers in Ultrafast Chiral Chromatography
  Daipayan Roy, Choyce A. Weatherly, M. Farooq Wahab, and Daniel W. Armstrong
  We explore the developments that have made it possible to produce sub-minute, and, more recently, even sub-second enantiomeric separations. We also look at the questions that remain unanswered.
  
• Biomimetic Chromatography to Accelerate Drug Discovery: Part II
  Klara Valko
  Biomimetic HPLC retention data can be used to measure how a compound will bind to proteins and phospholipids in vivo.
  
• Data Integrity in the Chromatography Laboratory, Part V: Second-Person Review
  Mark E. Newton and R.D. McDowall
  The series continues with a crucial scientific and regulatory necessity in ensuring reliable information—the second-person review.
  
• Chromatography Fundamentals, Part IV: Origin of Theoretical Plates—Fractional Distillation and Countercurrent Distribution Extractions
  Howard G. Barth
  The theoretical plate concept forms the basis of chromatographic theory. Here is where it came from.
  

DEPARTMENTS

• Peaks of Interest
• Products & Resources
• Calendar
• Short Courses
• Ad Index

COLUMNS

• COLUMN WATCH
  When Do We Need Sub-2-µm Superficially Porous Particles for Liquid Chromatography Separations?
  David S. Bell, Landon Wiest, Shun-Hsin Liang, and Dan Li
  Many manufacturers now offer columns using superficially porous particles that are 2-µm and smaller. When should you use them?
  
• LC TROUBLESHOOTING
  Tips, Tricks, and Troubleshooting for Separations of Biomolecules, Part I: Contemporary Reversed-Phase Protein Separations
  Szabolcs Fekete, Davy Guillarme, and Dwight R. Stoll
  For reversed-phase separations of proteins, you must consider pore size, column temperature, and stationary-phase chemistry. Here are some guidelines.
  
• GC CONNECTIONS
  Split, Splitless, and Beyond—Getting the Most from Your Inlet
  Nicholas H. Snow
  We discuss the challenges of split and splitless injections, ideas for mitigating them, and the case for renewed exploration of cool inlets and injection techniques.
  
• THE ESSENTIALS
  GC Column Maintenance: Tips for Extending GC Column Life
  To extend the life of your GC columns, follow these best practices.
  

PEER-REVIEWED ARTICLES

• Data Integrity in the GXP Chromatography Laboratory, Part IV: Calculation of the Reportable Results
  Mark E. Newton and R.D. McDowall
  You need to ensure that your calculations of reportable results don’t get you into data integrity trouble. Here’s how.
  
• Determination of Polycyclic Aromatic Hydrocarbons in Environmental Waters Using Heterogeneous Magnetic Materials Based on Metal–Organic Frameworks
  Priscilla Rocío-Bautista, Verónica Pino, Jorge Pasán, Juan H. Ayala, Catalina Ruiz-Pérez, and Ana M. Afonso
  This study of PAHs makes it easy to compare this microextraction procedure to conventional approaches and to other procedures using magnetic composites.
  
• Chromatography Fundamentals, Part III: Retention Parameters of Liquid Chromatography
  Howard G. Barth
  We review different approaches for measuring solute retention.
  
• Marjorie Groothuis Horning: Biochemist, Pharmacologist, and GC Pioneer
  Werner Engewald and Hartmut Frank
  A look back at this innovator’s career and her efforts to develop and popularize gas chromatography (GC), particularly for biomedical research.
  

DEPARTMENTS

• Peaks of Interest
• Chromatography Corner: Data-Independent Acquisition
• Chromatography Corner: Rapid Trace Analysis
• Calendar
• Short Courses
• Products & Resources
• Ad Index

COLUMNS

• COLUMN WATCH
  The Promise of Metal–Organic Frameworks for Use in Liquid Chromatography
  David S. Bell
  What can metal–organic frameworks offer for liquid chromatography?
  
• LC TROUBLESHOOTING
  Peak Purity in Liquid Chromatography, Part III: Using Two-Dimensional Liquid Chromatography
  Dwight R. Stoll, C.J. Venkatramani, and Sarah C. Rutan
  Here, we see how 2D-LC can solve coelution problems that are difficult or impossible to address using peak purity tools or curve resolution methods.
  
• PERSPECTIVES IN MODERN HPLC
  Antibody–Drug Conjugates: Perspectives and Characterization
  Rowan E. Moore, Kelly Broster, Ken Cook, Kyle D’Silva, Eric Niederkofler, Aaron O. Bailey, Jonathan Bones, and Michael W. Dong
  Comprehensive characterization of ADCs requires increasingly powerful approaches consisting of small- and large-molecule techniques.
  
• FOCUS ON BIOPHARMACEUTICAL ANALYSIS
  Analytical Characterization of Biotherapeutic Products, Part I: Quality Attributes
  Anurag S. Rathore, Ira S. Krull, and Srishti Joshi
  To ensure the reliable and accurate characterization of biotherapeutics, an arsenal of orthogonal analytical techniques is needed.
  
• THE ESSENTIALS
  HPLC Troubleshooting: Autosampler Contamination
  With autosamplers, we need to be extra careful to avoid contamination.
  

PEER-REVIEWED ARTICLES

• Profiling Nonionic Surfactants Applied in Pharmaceutical Formulations by Using Comprehensive Two-Dimensional LC with ELSD and MS Detection
  Gerd Vanhoenacker, Mieke Steenbeke, Koen Sandra, and Pat Sandra
  Comprehensive 2D-LC using HILIC and reversed-phase LC is a robust tool to characterize nonionic ethoxylated surfactants in pharmaceutical formulations.
  
• Chromatography Fundamentals, Part II: Thermodynamics of Liquid Chromatography: Energetics
  Howard G. Barth
  We examine the connection between the distribution coefficient and Gibbs free energy, and contributions from enthalpy and entropy.
  
• Biomimetic Chromatography to Accelerate Drug Discovery: Part I
  Klara Valko
  Drug discovery can be accelerated by chromatographic profiling of analogs by measuring their nonspecific binding to proteins and lipids.
  
• THE APPLICATION NOTEBOOK
  

DEPARTMENTS

• Peaks of Interest
• Products & Resources
• Ad Index

COLUMNS

• SAMPLE PREP PERSPECTIVES
  New Sample Preparation Products and Accessories
  Douglas E. Raynie
  Our yearly report on new products covers sample preparation instrumentation, supplies, and accessories. New sample preparation technologies introduced in the past year, while not necessarily disruptive, take giant leaps in that direction.
  
• LC TROUBLESHOOTING
  Fittings and Connections for Liquid Chromatography—So Many Choices!
  Dwight R. Stoll
  A bad connection between an LC column and the rest of the system can ruin a good separation. New technologies may improve the quality of these connections and the likelihood of establishing a good connection in the first place. Understanding the issues will help you choose the best option for you.
  
• GC CONNECTIONS
  New Gas Chromatography Products for 2017–2018
  John V. Hinshaw
  We present our annual review of new developments in the field of gas chromatography, which this year includes eight new GC and GC–MS laboratory benchtop systems as well as numerous new columns and accessories.
  
• THE ESSENTIALS
  A Step-by-Step Guide to Inlet Maintenance
  Good maintenance of the GC inlet can prevent a host of problems from compromising the quality of your results.
  

PEER-REVIEWED ARTICLES

• Quantitating Toxaphene Parlar Congeners in Fish Using Large Volume Injection Isotope Dilution GC with Electron-Capture Negative Ion MS
  Paul R. Loconto
  A novel automated ultratrace gas chromatography–mass spectrometry (GC–MS) method has been developed that quantitates the eight toxaphene Parlar congeners designated in U.S. Environmental Protection Agency Method 8276. This method, combined with an efficient extraction, cleanup, and fractionation technique, makes is possible to extend instrument detection limits to the low parts-per-trillion concentration level for these toxaphene Parlar congeners.
  
• Data Integrity in the GxP Chromatography Laboratory, Part III: Integration and Interpretation of Data
  Mark E. Newton and R.D. McDowall
  Integration is the heart of the chromatographic process and is subject to regulatory scrutiny. What should be done to control integration and interpretation of the chromatographic runs?
  

DEPARTMENTS

• Peaks of Interest
• Products & Resources
• Ad Index

COLUMNS

• COLUMN WATCH
  New Chromatography Columns and Accessories for 2018
  David S. Bell
  Our annual review of new liquid chromatography columns and accessories, including columns for reversed-phase, HILIC, chiral, SEC, GPC, ion-exchange, and SFC separations of small and large molecules.
  
• LC TROUBLESHOOTING
  Peak Purity in Liquid Chromatography, Part II: Potential of Curve Resolution Techniques
  Daniel W. Cook, Sarah C. Rutan, C.J. Venkatramani, and Dwight R. Stoll
  In part II of this series, we explore how curve resolution methods advance purity assessments and illustrate one of the most popular techniques, which adds a powerful tool to the chromatographer’s arsenal.
  
• PERSPECTIVES IN MODERN HPLC
  New HPLC Systems and Related Products Introduced in 2017–2018: A Brief Review
  Michael W. Dong
  An overview and assessment of the latest HPLC and mass spectrometry instruments, modules, chromatography data systems, and related software.
  
• FOCUS ON ENVIRONMENTAL ANALYSIS
  Best Practices for Analyzing Pesticides and Their Metabolites in Environmental Samples
  Laura Bush
  James Stry of FMC Agricultural Solutions talks about best practices for developing robust environmental analysis methods, including simplifying sample preparation and dealing with matrix effects.
  
• THE ESSENTIALS
  Making HILIC Work for You—Column Selection
  Ligands capable of undergoing electrostatic interactions can add an extra dimension to separations of ionizable compounds.
  

PEER-REVIEWED ARTICLE

• Data Integrity in the GxP Chromatography Laboratory, Part II: Setting up a Chromatograph and Acquiring Data
  Mark E. Newton and R.D. McDowall
  Part II of this series on practical perspectives on data integrity focuses on instrument setup, system suitability test samples, and data acquisition.
  

DEPARTMENTS

• Peaks of Interest
• Products & Resources
• Ad Index

COLUMNS

• SAMPLE PREP PERSPECTIVES
  Recent Advances in Solid-Phase Microextraction, Part I: New Tricks for an Old Dog
  Douglas E. Raynie
  A look at recent advances in SPME, such as increasing the sorbent surface area available for extraction, accommodating direct analysis by mass spectrometry, and sorbent overcoating to resist fouling by sugars and lipids
  
• LC TROUBLESHOOTING
  Eluent Preparation for Hydrophilic Interaction Liquid Chromatography, Part II: pH, Buffers, and Gradient Elution
  Dwight R. Stoll and Claudia Seidl
  Certain details related to mobile-phase preparation that can be assumed in reversed-phase LC separations can be much more consequential in HILIC.
  
• GC CONNECTIONS
  A Compendium of GC Detection, Past and Present
  John V. Hinshaw
  Gas chromatography makes use of a wide variety of detection methods, which really shine when deployed properly. Here’s guidance for how to choose the right one for your analysis.
  
• THE ESSENTIALS
  Optimizing SEC for Biologics Analysis
  Parameters such as pore size, column dimensions, temperature, flow rate, and mobile phase are important to consider when developing SEC methods.
  PEER-REVIEWED ARTICLES

PEER-REVIEWED ARTICLES

• Scaling LC Methods Using Superficially Porous Particle Stationary Phases
  Gregory K. Webster and Mathew A. Gragg
  Because not all laboratories have UHPLC systems, reverse scaling of methods from UHPLC to HPLC is often needed, particularly in the pharmaceutical industry. The use of superficially porous particles can facilitate this process.
  
• Chromatography Fundamentals, Part I: Thermodynamics of Liquid Chromatography: The Distribution Coefficient
  Howard G. Barth
  This article, the first in a series on chromatography fundamentals, discusses the cornerstone of all chromatographic techniques—the distribution or equilibrium coefficient—and its influence on liquid chromatographic separations.
  SPECIAL FEATURE

SPECIAL FEATURE

• Highlights of HPLC 2017 Jeju
  Ronald E. Majors
  A summary of the findings presented at the HPLC 2017 Jeju conference, reviewing how they fit into overall liquid-phase separation trends and the outlook for the future of these technologies
  

DEPARTMENTS

• Peaks of Interest
• Chromatography Corner
• Products & Resources
• Calendar
• Short Courses
• Ad Index

COLUMNS

• COLUMN WATCH
  Understanding the Science Behind Packing High-Efficiency Columns and Capillaries: Facts, Fundamentals, Challenges, and Future Directions
  Fabrice Gritti and M. Farooq Wahab
  Despite the theoretical promise of reduced plate heights (h) < 1, most modern UHPLC columns can only deliver plate heights in the range from 1.4 to 2.5. However, improved packing procedures, a better understanding of the colloidal properties of particle suspensions, and the study of the rheological behavior of packed beds and the final bed structure should lead us to practical solutions that can double the column efficiencies.
  
• LC TROUBLESHOOTING
  Peak Purity in Liquid Chromatography, Part I: Basic Concepts, Commercial Software, and Limitations
  Sarah C. Rutan, C.J. Venkatramani, and Dwight R. Stoll
  Is that peak “pure”? How do I know if there might be something hiding under there? In part I of this series, we explore some of the concepts behind peak purity assessments, describe some tools that are used in commercially available software for these assessments, and highlight some of the limitations of these tools using real-world examples.
  
• THE ESSENTIALS
  How to Avoid Problems in LC–MS
  Five tips to help you get the most out of your LC–MS instruments and methods
  

FEATURES

• The 2018 LCGC Awards
  Megan L’Heureux
  We explore the careers and achievements of the winners of LCGC’s 11th annual awards: Ronald E. Majors and Zachary S. Breitbach.
  
• Pittcon 2018: The LCGC Awards Symposium Preview
  In advance of Pittcon 2018, leading scientists—Ronald Majors, Richard Henry, John W. Dolan, Zachary S. Breitbach, and Daniel W. Armstrong—who will be speaking at the LCGC awards symposium give us a preview of their talks.
  

PEER-REVIEWED ARTICLE

• Accuracy Validation of Size-Exclusion Chromatography
  Howard G. Barth
  Here, a procedure is described for preparing polydisperse polymer standards to validate the accuracy of any SEC method for aqueous or organic mobile phases. This approach can be used for all calibration procedures with the exception of online light scattering and viscometric detection.
  

DEPARTMENTS

• Peaks of Interest
• Products & Resources
• Ad Index

COLUMNS

• SAMPLE PREP PERSPECTIVES
  Analyte Derivatization as an Important Tool for Sample Preparation
  Douglas E. Raynie
  There is a resurgence of interest in chemical derivatization schemes in separation science, particularly in sample preparation. Here’s why.
• LC TROUBLESHOOTING
  Eluent Preparation for Hydrophilic Interaction Liquid Chromatography, Part I: Solvent Volumes and Buffer Counterions
  Charles A. Lucy, Caley B. Craven, Claudia Seidl, and Dwight R. Stoll
  Paying attention to the details of mobile-phase preparation can have a big impact on the reproducibility of HILIC separations.
• FOCUS ON BIOPHARMACEUTICAL ANALYSIS
  Charge-Variant Profiling of Biopharmaceuticals
  Jared R. Auclair, Anurag Rathore, and Ira Krull
  A look at techniques for charge-variant analysis of monoclonal antibodies and the question of whether pH gradients are really better than salt gradients
• GC CONNECTIONS
  Tips and Tricks for New Gas Chromatographers
  Nicholas H. Snow
  Three main points summarize the best ways to be successful in GC: capillary GC is clean GC; practice, practice, practice; and be a student of GC.
• THE ESSENTIALS
  How It Works: Ion-Exchange SPE
  The fundamental principles of ion-exchange solid-phase extraction

PEER-REVIEWED ARTICLES

• Data Integrity in the GxP Chromatography Laboratory, Part I: Sampling and Sample Preparation
  Mark E. Newton and R.D. McDowall
  Part I of this series on practical perspectives of data integrity focuses on sample management, transport, and preparation.
• Headspace Solid-Phase Microextraction Coupled with Gas Chromatography–Mass Spectrometry for the Characterization of Polymeric Materials
  Peter Kusch
  HS-SPME-GC–MS is a valuable technique for identifying volatile organic compounds, additives, and degradation products in industrial rubber, car labeling reflection foil, and bone cement materials.

DEPARTMENTS

• Peaks of Interest
• Products & Resources
• Ad Index