COLUMNS
Column Watch
Highlights from HPLC 2015 Symposium
David S. Bell* and Xiaoli Wang†; *Sigma-Aldrich/Supelco and †Agilent Technologies
HPLC 2015, chaired by Gérard Hopfgartner was held in Geneva, Switzerland, from June 21–25. This installment covers some of the highlights observed at the symposium including stationary phase developments, particle technology, and areas of growing application of HPLC. In addition, trends and perspectives on future developments in HPLC culled from the conference are presented.
LC Troubleshooting
Column Problems Everywhere
John W. Dolan
No matter where you live or who you work for, you’re likely to encounter one or more of these LC column problems at some point.
MS—The Practical Art
Ion-Mobility Mass Spectrometry in Metabolomics and Lipidomics
Giuseppe Paglia and Giuseppe Astarita
Ion-mobility spectrometry (IMS) is an anlytical technique that provides for the separation of ions in the gas phase. The separation, occuring on a timescale of milliseconds, is based on the differing mobility of ions according to their charge, shape, and size. These characteristics make IMS suitable for coupling with mass spectrometry (MS), to serve in current MS-based workflows for metabolomics and lipidomics. IM-MS improves peak capacity and signal-to-noise ratios, and it provides more confidence during compound identification or confirmation than conventional analyses.
Biotechnology Today
Use of Sigmoidal Gradients in HPLC Based Analysis of Biotherapeutic Products
Anurag S. Rathore, Varsha Joshi, and Ira Krull
A systematic approach for formation of sigmoidal gradients has been discussed for analysis of biopharmaceutical proteins. The approach has been successfully demonstrated via two case studies. The first application involves HPLC separation of the various product-related variants of a microbial expressed biotherapeutic, granulocyte colony stimulating factor (GCSF). The second case study involves separation of the charge-heterogeneity related variants for two different monoclonal antibody (mAb) biotherapeutics. In all cases, it is observed that the use of sigmoidal gradient successfully reduces the analysis time significantly (from 70 min to 15 min for GCSF and from 40 min to 4 min for the mAbs) while retaining the selectivity and the resolution.
The Essentials
Sample Introduction for GC—Headspace Development and Optimization
Tony Taylor and John Hinshaw
Improve your headspace sampling methods through a deeper understanding of the effects of key method parameters
ARTICLE
Method Development and Validation of Trace Levels of Carbon Tetrachloride in Flunixin Meglumine by Headspace Gas Chromatography with Flame Ionization Detection
S. Natarajan* and B.K. Kempegowda†, *Bharathiar University, India; †Maharani's Science College for Women, India
A simple and accurate method was developed using gas chromatography for determining the trace level of the carcinogenic solvent carbon tetrachloride (CCl4) in flunixin meglumine, a white crystalline powder drug substance. The method was observed to be robust and complete analytical method validation determined that it meets ICH requirements. The method has a lower limit of detection than those of other methods currently available. The method was implemented for various active pharmaceutical ingredients (API) successfully.
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