LC*GC

December 2011
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Volume 29, Number 12, December 2011
LC*GC December 2011 Table of Contents
COLUMNS
- SAMPLE PREP PERSPECTIVES
Hollow-Fiber Liquid-Phase Microextraction in the Three-Phase Mode - Practical Considerations
Astrid Gjelstad, Hamidreza Taherkhani, Knut Einar Rasmussen, and Stig Pedersen-Bjergaard
The practical aspects of hollow-fiber liquid-phase microextraction in the three-phase mode (HF3LPME) are described.
- LC TROUBLESHOOTING
Troubleshooting Basics, Part III: Retention Problems
John W. Dolan
A look at situations in which retention times are too long, too short, or inconsistent
- BIOTECHNOLOGY TODAY
Current Applications of UHPLC in Biotechnology, Part II: Proteins and Glycans
I.S. Krull, A. Rathore, and Thomas E. Wheat
A discussion of how UHPLC is used to conduct intact protein-antibody analysis and glycoprofiling to characterize biopharmaceutical drugs
ARTICLES
- Analysis of Phenazepam in Whole Blood Using Solid-Phase Extraction and LC-Tandem Mass Spectrometry
Albert A. Elian, Jeffery Hackett, and Michael J. Telepchak
Phenazepam is becoming a drug of interest in forensic laboratories. This new procedure will enable forensic toxicologists to analyze phenazepamin biological fluids quickly and easily.
- 2011 Editorial Index
LCGC North America provides its annual editorial index, organized by authors and subjects.
DEPARTMENTS
- Peaks of Interest
- Product Resources
- Ad Index
Volume 29, Number 11, November 2011
LC*GC November 2011 Table of Contents
COLUMNS
- SAMPLE PREP PERSPECTIVES
Prevention Is Better than Cure: An Alternative Approach for the Sample Preparation of Complex Samples
Precious Sibiya, Ewa Cukrowska, and Luke Chimuka
Combining a membrane with a solid sorbent can improve selectivity and save time in sample preparation.
- LC TROUBLESHOOTING
Locating Precision Problems
John W. Dolan
Do you have too much variability in your liquid chromatography method? Here's how to track down the source of the problem.
- GC CONNECTIONS
Valves for Gas Chromatography, Part III: Fluidic Switching Applications
John V. Hinshaw
How to use fluidic switching devices for open-tubular column manipulations, such as heartcutting and comprehensive multidimensional GCxGC.
- HISTORY OF CHROMATOGRAPHY
John Knox, a Pioneer of Both Gas and Liquid Chromatography
Gert Desmet
An interview with John Knox, who brought us the Knox equation, porous graphite carbon, and other critical advances in both liquid and gas chromatography.
ARTICLE
- A Simple Instrumental Approach for "Supercritical" Fluid Chromatography in Drug Discovery and Its Consequences for Coupling with Mass Spectrometric and Light Scattering Detection
Alberto Pereira, Frank David, Gerd Vanhoenacker, ClaudioBrunelli, and Pat Sandra
A simple experimental setup applied in a drug discovery laboratory illustrates some anomalies and misconceptions about supercritical fluid chromatography for drug discovery.
DEPARTMENTS
- Peaks of Interest
- Product Resources
- Literature
- Ad Index
Volume 29, Number 10, October 2011
LC*GC October 2011 Table of Contents
COLUMNS
- COLUMN WATCH
A Systematic Study of Achiral Stationary Phases Using Analytes Selected with a Molecular Diversity Model
Ray McClain and Matt Przybyciel
A limited set of stationary phases can separate a wide variety of molecules and maintain good peak shape without mobile-phase additives.
- LC TROUBLESHOOTING
Column Triage
John W. Dolan
How do you react to symptoms that indicate your liquid chromatography column has major problems?
- GC CONNECTIONS
Headspace Sampling
John V. Hinshaw
A clear understanding of the chemical system of the sample in headspace - and how temperature and peak volume affect peak areas, sensitivities, and repeatability - will improve headspace analysis.
- INNOVATIONS IN HPLC
Nano LC: Principles, Evolution, and State-of-the-Art of the Technique
Laurent Rieux, Evert-Jan Sneekes, and Remco Swart
Nano LC is now widely applied in proteomics, and also is robust enough for application in fields such as pharmaceutical analysis.
ARTICLE
- Laser Diode Thermal Desorption Tandem Mass Spectrometry for Simultaneous Quantitation of Metformin and Sitagliptin in Mouse and Human Dried Blood Spots
John G. Swales, Richard T. Gallagher, Mark Denn, Raimund M. Peter, and Nick Duczak
An exploration of LDTD-MS-MS and how it compares to HPLC-MS-MS techniques in terms of sensitivity, robustness, and speed in an in-vivo drug discovery application
DEPARTMENTS
- Peaks of Interest
- Product Resources
- Ad Index
Volume 29, Number 9, September 2011
LC*GC September 2011 Table of Contents
COLUMNS
- COLUMN WATCH
Highlights of HPLC 2011
Ronald E. Majors
A presentation of the overall trends in liquid-phase chromatography observed at the symposium, as well as the awards presented and the opening plenary session
- LC TROUBLESHOOTING
Troubleshooting Basics, Part II: Pressure Problems
John W. Dolan
A look at ways to estimate what normal system pressure should be and some likely causes of various pressure abnormalities
- MS - THE PRACTICAL ART
Visualizing the Chemical Composition of Complex Samples
Michael P. Balogh and David Stranz
How does one decipher and tabulate thousands of chemical formulas and relative abundances without losing the important details?
- BIOTECHNOLOGY TODAY
Current Applications of UHPLC in Biotechnology, Part I: Peptide Mapping and Amino Acid Analysis
I.S. Krull, A. Rathore, and Thomas E. Wheat
A description of the use of UHPLC in the biopharmaceutical industry to characterize drug substances through peptide mapping and amino acid analysis
ARTICLES
- Analysis of Psilocybin and Psilocin in Urine Using SPE and LC-Tandem Mass Spectrometry
Albert A. Elian, Jeffery Hackett, and Michael J. Telepchak
An SPE procedure is described that isolates both psilocybin and psilocin from urine samples for LC-MS-MS analysis.
- Trace Metabolic Profiling and Pathway Analysis of Clomazone Using LC-MS-MS and High-Resolution MS
Wei Zou, Hagai Yasuor, Albert J. Fischer, and Vladimir V. Tolstikov
A novel approach for detection, analysis, and characterization of low-abundant herbicide metabolites is reported here.
DEPARTMENTS
- Peaks of Interest
- Product Resources
- Calendar
- Short Courses
- Chrom Corner
- Ad Index
Volume 29, Number 8, August 2011
LC*GC August 2011 Table of Contents
COLUMNS
- COLUMN WATCH
The State of the Art in Chiral Capillary Gas Chromatography
Thomas Beesley
A brief history of phase development is presented, along with a comparison of gas chromatography and high performance liquid chromatography chiral separations.
- LC TROUBLESHOOTING
How Fast Can a Gradient Be Run?
John W. Dolan
An exploration of how different variables affect a separation.
- HISTORY OF CHROMATOGRAPHY
My Mentors, Colleagues, and Friends in Separation Science and Technology, Part II
Klaus K. Unger
This final installment of Klaus Unger's personal reflections and scientific activities covers from 1990 until his retirement in 2010.
ARTICLES
- The Effect of SEC Column Arrangement of Different Pore Sizes on Resolution and Molecular Weight Measurements
Bruce Kempf, Roy Eksteen, and Howard G. Barth
The results of a study to determine the influence of SEC column order on molecular size separation and peak broadening.
- Determination of α-Amanitin in Human Serum by Solid-Phase Extraction Coupled with HPLC-UV
Zhi Zhou, Min Cao, Liping Zhou, Xiongjun Zuo, and Youwen Tang
A method is presented for the determination of -amanitin, a toxic cyclic octapeptide of amanitin mushrooms, in human serum by solid-phase extraction coupled with high performance liquid chromatography with UV detection.
- Generous Results with MISER Chromatography
Alasdair Matheson
An interview with Merck's Christopher Welch about highthroughput analysis using MISER chromatography and how it can boost your laboratory's productivity.
DEPARTMENTS
- Peaks of Interest
- Product Resources
- Literature
- Calendar
- Info for Authors
- Ad Index
Volume 29, Number 7, July 2011
LC*GC July 2011 Table of Contents
COLUMNS
- COLUMN WATCH
Method Translation in Gas Chromatography
Ronald E. Majors and Ken Lynam
Method translation software enables conversion and improvement of GC methods.
- LC TROUBLESHOOTING
Troubleshooting Basics, Part I: Where to Start?
John W. Dolan
Rules of thumb for isolating problems, determining problem sources, and developing a maintenance routine.
- GC CONNECTIONS
Valves for Gas Chromatography, Part II: Applications
John V. Hinshaw
Discussion about the use of gas switching valves for column backflush and two-dimensional series-bypass applications.
- INNOVATIONS IN HPLC
Pulsed Electrochemical Detection: Waveform Evolution
William R. LaCourse
Developments in pulsed electrochemical detection are traced through the progression of its waveforms.
ARTICLES
- Improving the Efficiency of Fatty Acid Methyl Ester Preparation Using Automated Sample Preparation Techniques
Rebecca A. Veeneman
An automated technique for esterifying fatty acids in canola oil compares favorably with a manual method.
- Determination of Clenbuterol-Like Beta-Agonist Residues in Hair
Wan-hua Yang, Wen-ting Ling, Qin Fen, and Gui-liang Chen
LC-MS-MS is used to detect compounds relevant for food safety.
- Electrostatic Repulsion-Hydrophilic Interaction Chromatography: Using One Mode to Tune Retention from a Second Mode
Andrew Alpert and Amos Heckendorf
Electrostatic effects superimposed on hydrophilic interactions enables selection or deselection of functional groups for compound isolation.
- On-Line Whole Blood Analysis Using Microextraction by Packed Sorbent and LC-MS-MS
Mohamed Abdel-Rehim
A new sample preparation method is described for whole blood sample analysis in clinical and preclinical studies.
DEPARTMENTS
- Peaks of Interest
- Product Resources
- Literature
- Calendar
- Short Courses
- Ad Index
Volume 29, Number 6, June 2011
LC*GC June 2011 Table of Contents
COLUMNS
- COLUMN WATCH
Method Translation in Liquid Chromatography
Ronald E. Majors
Converting a method from conventional HPLC to high-throughput HPLC or UHPLC is easy with a method translation calculator. Here's how to use them and where to find them, for free.
- LC TROUBLESHOOTING
The Case of the Too Big Little Peak
John W. Dolan
A case of over-recovery of a preservative on ageing of a pharmaceutical product provides a good example of how to approach solving a problem of overlapping peaks in an LC separation.
- MS - THE PRACTICAL ART
Testing the Critical Interface: Leachables and Extractables
Michael P. Balogh
Coping with extractables and leachables testing is easier when you have a good understanding of the issues involved. Information from public databases and industry consortia also is invaluable.
- BIOTECHNOLOGY TODAY
Biotechnology Highlights from Isranalytica 2011
Ira S. Krull, Anurag S. Rathore, and Simion Kreimer
Isranalytica offered great talks on biotechnology, on topics from comprehensive protein characterization to middle-out proteomics to capillary electrophoresis for glycoprofiling.
ARTICLE
- Why All C18 SPE Phases Are Not Equal
Craig A. Perman and Michael Telepchak
Octadecyl bonded silica gel (C18) is widely used in solid-phase extraction (SPE), but there are many variations including particle size, pore size, surface chemistry, and carbon loading applications.
DEPARTMENTS
- Peaks of Interest
- Product Resources
- Literature
- Calendar
- Ad Index
Volume 29, Number 5, May 2011
LC*GC May 2011 Table of Contents
COLUMNS
- COLUMN WATCH
Self-Assembled Nanomaterials for Enhanced Chemical Separations
Stephanie A. Archer-Hartmann and Lisa A. Holland
Nanomaterials offer exciting possibilities for improving separations with techniques such as TLC, SPME, and CE.
- LC TROUBLESHOOTING
Ghost Peak Investigation in a Reversed-Phase Gradient LC System
Silvia Sadikin, Dee Dee Zhang, Roger Inloes, and Sanjeev Redkar
Here is a step-by-step approach to investigate the source of ghost peaks in a gradient LC method.
- GC CONNECTIONS
New Gas Chromatography Products at Pittcon 2011
John V. Hinshaw
This was a strong year for GC systems. Here's what is new.
- INNOVATIONS IN HPLC
HPLC Systems and Components Introduced at Pittcon 2011: A Brief Review
Michael Swartz
This year, many HPLC systems focused on facilitating process development, method transfer, and biological analysis.
ARTICLES
- Establishing USP Rebaudioside A and Stevioside Reference Standards for the Food Chemicals Codex
Yi Dang, Jeffrey Moore, Gloria Huang, Markus Lipp, Barbara Jones, and James C. Griffiths
Here's how these new reference standards were characterized.
- A Generic Workflow for Achiral SFC Purification of Complex Pharmaceutical Mixtures
Vivi Lazarescu, Mark J. Mulvihill, and Lifu Ma
This process can improve efficiency in a drug discovery laboratory.
DEPARTMENTS
- Peaks of Interest
- Product Resources
- Literature
- Calendar
- Short Courses
- Ad Index
Volume 29, Number 4, April 2011
LC*GC April 2011 Table of Contents
COLUMNS
- COLUMN WATCH
New Chromatography Columns and Accessories at Pittcon 2011: Part II
Ronald E. Majors
A review of the gas chromatography columns, sample preparation, and chromatographic and sample preparation accessories that were presented at Pittcon 2011.
- LC TROUBLESHOOTING
Selectivity in Reversed-Phase LC Separations, Part IV: Pressure Selectivity
John W. Dolan
Can pressure alone affect the appearance of a chromatogram?
- THE HISTORY OF CHROMATOGRAPHY
My Mentors, Colleagues, and Friends in Separation Science and Technology, Part I
Klaus K. Unger
Often, what you remember most about your career is the great people you met along the way.
ARTICLES
- Determination of Phenylurea Herbicides in Tap Water and Soft Drink Samples by HPLC-UV and Solid-Phase Extraction
Manpreet Kaur, Ashok Kumar Malik, and Baldev Singh
A high performance liquid chromatography (HPLC)-UV method was developed for the analysis of phenylurea herbicides and applied successfully to the analysis of herbicides spiked in three soft drink brands and tap water.
- Development and Validation of an HPTLC Method for Determination of Aflatoxin B1
Hegang Gao, Li Chen, Guoshao Pan, and Chunyu Tu
A high performance thin-layer chromatographic (HPTLC) method was developed for the determination of aflatoxin B1 in cereals.
DEPARTMENTS
- Peaks of Interest
- Product Resources
- Literature
- Calendar
- Ad Index
Volume 29, Number 3, March 2011
LC*GC March 2011 Table of Contents
COLUMNS
- COLUMN WATCH
New Chromatography Columns and Accessories at Pittcon 2011: Part I
Ronald E. Majors
A review of the liquid chromatography columns and accessories for analytical and preparative chromatography to be unveiled at Pittcon 2011.
- LC TROUBLESHOOTING
Selectivity in Reversed-Phase LC Separations, Part III: Column-Type Selectivity
John W. Dolan
Comparisons between different C18 columns and the best way to select which one to use.
- GC CONNECTIONS
Valves for Gas Chromatography: Fundamentals
John V. Hinshaw
The first installment in this series on valves presents basic concepts, applications, and implementations.
- BIOTECHNOLOGY TODAY
High-Throughput Tools and Approaches for Development of Process Chromatography Steps
Anurag S. Rathore, Rahul Bhambure, and Ira S. Krull
An overview of high-throughput process development (HTPD) tools and approaches, as well as a case study.
ARTICLES
- The 2011 LCGC Pittcon Awards
Laura Bush
The winners of LCGC's fourth annual awards, who will be honored at Pittcon 2011 and interviewed in the LCGC Pittcon Theater.
- HILIC-MS Sensitivity without Silica
Luisa Pereira
What challenges occur when using hydrophilic interaction liquid chromatography (HILIC), and what options are available for analysis?
- The Secrets of Electrospray Ionization: Why Less is More
An interview with Kevin Schug of the University of Texas at Arlington.
DEPARTMENTS
- From the Editor
- Peaks of Interest
- Product Resources
- Literature
- Calendar
- Ad Index
Volume 29, Number 2, February 2011
LC*GC February 2011 Table of Contents
COLUMNS
- SAMPLE PREP PERSPECTIVES
The Greening of the Chromatography Laboratory
Ronald E. Majors and Douglas Raynie
Miniaturization and solvent substitution are two key approaches.
- LC TROUBLESHOOTING
A Picture Is Worth a Thousand Words
Kasper Pedersen and John W. Dolan
A few simple calculations and estimates can provide insight into a troublesome chromatogram.
- MS-THE PRACTICAL ART
Problem Solving in the Chemical Industry
Michael P. Balogh
Identifying unknown compounds continues to challenge analysts.
- THE HISTORY OF CHROMATOGRAPHY
Still a Young Technology, Chiral Chromatography Makes Big Strides in Pharma
Pilar Franco
Chiral chromatography is now the fastest way to access large amounts of enantiopure pharmaceutical compounds.
ARTICLES
- A Rapid and Space-Saving Method for Determining Melamine in Milk Under Organic Solvent-Free Conditions
Naoto Furusawa
High recovery, reproducibility, and cost savings are among the advantages of this environmentally friendly method.
- Aggregated Singletons for Automated Purification Workflow
Bhagyashree A. Khunte and Laurence Philippe
A multistep workflow process provides purified samples for in-vitro testing in just two or three business days.
- An Emerging Leader: One Year Later
Megan Evans
An interview with Jared Anderson of the University of Toledo.
DEPARTMENTS
- From the Editor
- Peaks of Interest
- Pittcon Showcase
- Literature
- Calendar
- Short Courses
- Ad Index
Volume 29, Number 1, January 2011
LC*GC January 2011 Table of Contents
COLUMNS
- SAMPLE PREP PERSPECTIVES
New Directions in Whole Blood Analysis: Dried Blood Spot Analysis and Beyond
Ronald E. Majors
New methods are available for whole blood analysis. Here, various approaches are compared and contrasted.
- LC TROUBLESHOOTING
Selectivity in Reversed-Phase LC Separations, Part II: Solvent-Strength Selectivity
John W. Dolan
This month's "LC Troubleshooting" looks at the regular changes in retention that are observed with a change in the solvent strength and how to take advantage of them during method development.
- GC CONNECTIONS
Hydrogen Carrier Gas and Vacuum Compensation
John V. Hinshaw
John Hinshaw investigates the influence that choosing hydrogen carrier has on column selection and operation with direct-interface GC-MS.
- VALIDATION VIEWPOINT
Analytical Method Validation: Back to Basics, Part II
Michael Swartz and Ira Krull
The authors discuss the specifics of analytical method validation.
ARTICLES
- The Direct Analysis of Diquat and Paraquat in Lake Water Samples by per Aqueous Liquid Chromatography
Christina S. Robb and Brian D. Eitzer
The authors discuss an LC method for the direct analysis of diquat and paraquat in lake water.
- Quantification of Total ω-6 and ω-3 Fatty Acids and ω-6/ω-3 Ratio in Human Serum Using GC-MS
Mary W. Muriuki, Gerard G. Dumancas, Neil Purdie, and Lisa Reilly
The article demonstrates the superiority of the GC-MS approach over spectrophotometry.
- Toward a Universal Detector for Small Molecule Applications: Direct-EI in LC-MS
Pierangela Palma, Giorgio Famiglini, Helga Trufelli, and Achille Cappiello
The potential of direct-EI is illustrated with a selection of practical applications.
- Optimization of Asymmetrical Flow Field-Flow Fractionation
Rashid N. Qureshi and Wim Th. Kok
This article illustrates how to choose the best experimental parameters for asymmetrical flow field-flow fractionation.
DEPARTMENTS
- Peaks of Interest
- Product Resources
- Literature
- Calendar
- Short Courses
- Ad Index