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Special Issues

Systematic toxicological analysis is an important step in medicolegal investigations of death, poisoning, and drug use. The primary goal is the detection and confirmation of potentially toxic compounds in evidence. This article describes a workflow using nontargeted liquid chromatography–tandem mass spectrometry (LC–MS/MS) for reliable compound identification.

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LCGC Europe

In his final column before retirement, John Dolan reminisces about his years as the author of “LC Troubleshooting”, and some of the changes that have taken place in liquid chromatography (LC) technology during that time.

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LCGC Europe

Separating proteins and antibodies is a unique analytical challenge because of the complexity of the analytes. Both sample heterogeneity, because of a number of chemical modifications to the analyte, and nonspecific binding to the silica surface often result in chromatographic peak broadening and tailing. This instalment of “Column Watch” focuses on several different chromatographic strategies that analytical scientists can use to resolve and quantitate various biomacromolecules, including monoclobal antibodies (mAbs) and antibody–drug conjugates (ADCs). Selected aspects of size-exclusion, hydrophobic interaction, ion-exchange, hydrophilic interaction, and reversed-phase chromatography are discussed.

Internal standards (IS) are commonly incorporated into quantitative methods to increase accuracy and precision. An IS is a compound that is different than the analyte of interest, has similar physicochemical properties to the analyte, and is added to samples, calibration standards, and quality control samples in a known quantity. It should not be present in the sample, it should be available in high purity, and it should be easily differentiable from the analyte of interest.

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Digital Watch

The Column

Incognito wonders where we are, where we have been, and where we are going digitally in the analytical laboratory.

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The Column

Researchers from the University of Torino have developed a novel HPLC–HRMS application for evaluating cosmetic ingredient composition. The application was used to analyze and compare sturgeon eggs, commonly known as caviar, and brill eggs, and their use in beauty creams as lipid sources.

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The Column

Capillary electrophoresis (CE) is routinely used for chemical and biochemical analysis methods, and recently the technique has been implemented on microchips. R. Scott Martin, a professor and chair of chemistry at Saint Louis University, St. Louis, Missouri, USA, has been investigating ways to improve these techniques for years. He recently spoke to us about his research coupling microchip electrophoresis with electrochemical detection, coupling continuous flow with microchip electrophoresis with valving, coupling microchip CE with microdialysis sampling and electrochemistry, and more.

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The Column

The ability to rapidly screen stationary phases through column-switching capabilities provides significantly greater efficiency in method development than was previously possible. The approach does require some additional hardware and software. And, while such capabilities may limit the ability to expand one’s literary knowledge during excessive months in the laboratory developing separation methods, real progress to key decision points for method optimization can be realized instead.

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LCGC Asia Pacific

Small differences in process gas chromatography (GC) results from the same sample stream over time can indicate corresponding changes in target analyte concentrations, or the fluctuations might be due to external influences on the instrument. This instalment of ”GC Connections” explores ways to examine such results and better understand their significance.

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LCGC Asia Pacific

Using a liquid chromatography–mass spectrometry (LC–MS) method in conjunction with two complementary types of chromatographic retention modes-reversed phase and aqueous normal phase-various compounds present in mesquite flour extracts were identified. Because of the diverse types of chemical constituents found in such natural product extracts, a single chromatographic mode may not be sufficient for a comprehensive characterization. However, the combination of reversed-phase and aqueous normal phase LC can encompass a wide range of analyte polarity. This characterization of the composition of mesquite flour could be used in future studies to elucidate the beneficial health effects of its consumption.

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LCGC Europe

In the previous instalment, we presented a case of periodically fluctuating data that did not lend itself well to trend analysis with conventional statistical methods. The data did appear to have a strong regular fluctuation, but its relationship to other observations was not clear. This instalment addresses methods for teasing out external influences on trending data.

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LCGC Europe

The 45th International Symposium on High Perfomance Liquid Phase Separations and Related Techniques (HPLC 2017), cochaired by Michal Holc€apek and František Foret, was held 18–22 June in Prague, Czech Republic. This instalment covers some of the highlights observed at the symposium, including advances in large-molecule separations, multidimensional chromatography, and areas of growing application of high performance liquid chromatography (HPLC). In addition, trends and perspectives on future developments in HPLC noted from the conference are presented.

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The Application Notebook

Polybrominated diphenyl ethers (PBDEs) are a worldwide contamination problem. Structurally similar to polychlorinated biphenyl (PCBs), these compounds are long-lived in the environment and can bioaccumulate throughout the food chain. The health hazards of these chemicals have attracted increasing scrutiny and, as such, a great deal of research and regulations have been implemented to manage and control them.

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The Application Notebook

Perfluorinated alkyl acids are man-made fluorochemicals used as surface-active agents in the manufacture of a variety of products, such as firefighting foams, coating additives, textiles, and cleaning products. They have been detected in the environment globally and are used in very large quantities around the world. These fluorochemicals are extremely persistent and resistant to typical environmental degradation processes. As a result, they are widely distributed across the higher trophic levels and are found in soil, air, groundwater, municipal refuse, and landfill leachates. The toxicity, mobility, and bioaccumulation potential of perfluorooctanesulfonic acid (PFOS) and perfluorooctanoic acid (PFOA), in particular, pose potential adverse effects for the environment and human health.