HPLC and GC Articles

In previous columns I have mainly discussed aspects of method validation for product analysis performed in quality control (QC) laboratories, but not for bioanalytical methods. To be specific, a bioanalytical method in the context of this column is the analysis of small drug molecules and any metabolites in biological samples generated from non-clinical and clinical studies.

In the 1950s, petroleum-related gas chromatography mass spectrometry (GC–MS) applications were one of the founding cornerstones of modern mass spectrometry.

There seem to be a disproportionate number of problems encountered in the concentration region near the limit of detection (LOD) and lower limit of quantification with calibration curves used for liquid chromatography (LC) methods. Some of these problems relate to improperly selecting the model used for calibration.

Chromatographic resolution of pharmaceutical compounds is one of the most efficient approaches for generating small quantities of pure material for biological testing in early pharmaceutical research and development (1–3). The use of chromatographic resolution from a purification group allows more time for synthetic chemists to make more compounds for research.

Quality-by-design (QbD) is a methodology gaining widespread acceptance in the pharmaceutical industry. A core tenet of this methodology is the idea of establishing the design space of a product or process as a primary R&D goal. Many articles have been published recently describing the successful application of QbD to process development.

In the 1950s, petroleum-related gas chromatography–mass spectrometry (GC–MS) applications were one of the founding cornerstones of modern MS. Even now, "petroleomics" — not to be outdone by life science research — serves as an example of the cutting edge in liquid chromatography–mass spectrometry (LC–MS) (1).

This is the second installment in a series of "LC Troubleshooting" articles on calibration curves for liquid chromatography (LC) separations. Last month's column (1) looked briefly at single-point, two-point, and multipoint calibration curves.

Pittcon 2009, the 60th Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy, was held in the massive McCormick Place in Chicago, Illinois, on March 8–13, 2009, the sixth time the Conference has been held there. This year's event hosted nearly 1000 instrument manufacturers and laboratory suppliers in more than 2200 booths.

Recently, I had the opportunity to participate in Colacro XII, a chromatography symposium held in a Latin America country every two years. This year's meeting was held in Florianopolous, Brazil, 27–30 October. During the symposium, I perused the large number of applications posters for the sample preparation techniques being used.

Often, one of the first signs of trouble with a liquid chromatography (LC) method is a failure to pass the system suitability requirements for the method. In fact, early warning of potential problems is one of the primary purposes of a system suitability test.