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This article reports on the physical phenomena that control column efficiency and on experimental protocols designed to accurately measure their contributions to band broadening of analytes during their passage from the injection to the detection device. The results of these protocols are analyzed, allowing for the accurate determination of the complete mass transfer mechanism in different separation modes and providing solutions and future directions to further improve the efficiency of liquid chromatography columns.  

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Alzheimer's Disease (AD) is one of the most common neurodenerative disorders worldwide. It is a progressive disorder characterized by gradual loss of mental ability associated with the death of brain cells, and is diagnosed using a combination of physical, neurological, and laboratory tests. Although there are no curative treatments available, early treatment can reduce the rate of the disease progression. Scientists from the University of Huelva and the Neurological Service from the Hospital Juan Ramon Jim?nez in Spain, began collaborating four years ago to develop new strategies to identify biomarkers that could be used to speed up diagnosis of the disease. In a new study published in the journal Electrophoresis, the team present a metabolomics approach based on ultrafiltration followed by capillary electrophoresis coupled with mass spectrometry (CE–ESI–MS) for the fingerprinting of polar metabolites in blood serum.

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The production of new drugs continues to increase, placing pressure on analytical scientists to develop new bioanalytical methods to characterize and ensure quality control and safety. Bethany Degg of The Column spoke to Lucie Novakova of Charles University in Prague, Czech Republic, about the development, optimization, and challenges of bioanalytical methods as well as future emerging research areas.

Back to Basics

Incognito goes back to basics with standard laboratory skills. How do you use your pipette properly?

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Researchers from CSIRO Oceans and Atmosphere Flagship in Hobart, Australia, have published a new approach to monitoring plastic exposure in live birds. Featured in the journal Methods in Ecology and Evolution, the study describes the sampling of preen oil collected from seabirds using a simple swabbing method for gas chromatography coupled to mass spectrometry (GC–MS) analysis.1

Much has been written about options for increasing efficiency in HPLC ? primarily through the use of core shell and sub 2 ?m particles, which have been used to increase efficiency, speed up separations or increase peak capacity. However, many separations can only be effectively improved, by optimising selectivity ? resolution is a function of selectivity, efficiency and retention, with selectivity being the most effective at achieving good resolution.

I will preface this blog installment by saying that I am not an expert on separation of proteins, but I am learning. What I do understand are the fundamentals of chromatography for small molecules. This information abounds, but it is much more difficult to find the same level of information for biomacromolecule chromatography.

Richard Henry discusses what chromatographers need to learn, from measuring dispersion and using Van Deemter and Van 't Hoff plots to getting familiar with mobile phase variables.

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There are over 100 different types of vanilla, all characterized by different aroma profiles. To determine vanilla origin, and for quality control purposes, laboratories typically rely on headspace or thermal desorption techniques used in combination with gas chromatography–mass spectrometry (GC–MS). This article explains more.

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A new study published in the journal Analytical Chemistry by scientists from the University of California Davis, the National Marine Mammal Foundation, and the Chicago Zoological Society in the USA presents a novel breath analysis method for Atlantic bottlenose dolphins (Tursiops truncatus) that could be used to monitor and assess the health of wild marine mammal populations.

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A team of researchers at the University of Huddersfield, UK, has investigated the potential of okra for emulsification of certain food products using size-exclusion chromatography (SEC) and fourier transform infrared (FTIR) spectroscopy.1 Okra is a flowering plant and originates from Africa. Okra pectins are acidic, random coil polysaccharides composed of galactose, rhamnose, and galacturonic acid. Pectins are used in the food industry for their gelling, stabilizing, and thickening properties. Okra pectins differ quite substantially from those extracted from apple, citrus, and beet in terms of protein and acetyl contents, indicating their greater hydrophobicity and suggesting that pectin derived from okra can be used as an effective emulsifying agent.?

Scientists from the Helmholtz Centre for Environmental Research in Germany, have developed a high performance liquid chromatography tandem mass spectrometry (HPLC–MS–MS) method to determine the internal concentrations of 34 test compounds in zebrafish (Danio rerio) embryos.

Professor Georges Guiochon, Distinguished Professor at the University of Tennessee in Knoxville, USA sadly passed away last week on October 21st 2014 at the age of 83. Professor Guiochon was a famous and flamboyant figure in the chromatography community with a prolific output that led to a deeper understanding of the separation mechanisms involved in chromatography.