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Lourdes Ramos

Latest:

Sample Preparation: The State of the Art

In this extended special feature to celebrate the 30th anniversary edition of LCGC Europe, leading figures from the separation science community explore contemporary trends in separation science and identify possible future developments. We asked key opinion leaders in the field to discuss the current state of the art in sample preparation.



Hernan Cortes

Latest:

Multidimensional Gas Chromatography using Planar Microfluidic Devices for the Characterization of Chlorinated Degreasers in Marine Gas Oil

A practical and reliable analytical procedure that incorporates MDGC with a planar microfl uidic device as a Deans switch was developed for the characterization of chlorinated degreasers in marine gas oil.


A. Talamona

Latest:

Isolation of Benzylideneacetophenone from a Crude Reaction Mixture

Benzylideneacetophenone forms the central core for a variety of important biological compounds, known collectively as chalcones. Many of these compounds have significant medicinal value as they demonstrate antibacterial, antifungal, antitumor, and anti-inflammatory properties.


Hannah Calder

Latest:

Detection of ODSs and HGSs in Industrial Zones Using a Cryogen-Free Preconcentration GC–MS Method

Adopted 35 years ago, the Montreal Protocol is an international treaty designed to protect the ozone layer. It addresses ozone depletion caused by industrial chemicals and remains a landmark environmental agreement in the phasing out and ban of the production and consumption of ozone-depleting substances (ODSs).


Ludivine Fromentoux

Latest:

Determination of Contaminants in Beer Using LC–MS/MS and ICP-MS

The German Beer Purity Law of 1516 makes beer one of the best analyzed food products with the highest standards regarding quality, freshness, appearance, and flavor. According to this law, beer is allowed to contain hops, malt, yeast, and water as ingredients. Of course, beer also contains major B vitamins, bitter substances, and minerals and trace elements (such as Ca, Na, Mg, and Zn) that are important for human nutrition. However, undesirable substances such as pesticides and heavy metals (for instance Cd, Pb, Hg, Sb, and As) can be found as well, mostly as contaminants in brewing water and grains. In particular, the herbicide glyphosate has to be monitored carefully since it is discussed as a possible carcinogenic. The chromatography of glyphosate is challenging because of its high polarity. A well-established method including a derivatization step with 9-fluorenylmethyl chloroformate (FMOC) followed by LC–MS analysis is time-consuming and also susceptible to errors. A sample pretreatment without derivatization is desirable because it is faster and cheaper. A triple quadrupole mass spectrometer optimizes the analytical procedure and establishes a routine method for the analysis of glyphosate in beer. For the determination of low element concentrations, such as As, Se, Pb, Cd, and Zn, inductively coupled plasma-mass spectrometry (ICP-MS) is applied.


Gottfried Reznicek

Latest:

Workflow Development for the Analysis of Phenolic Compounds in Wine Using Liquid Chromatography Combined with Drift-Tube Ion Mobility–Mass Spectrometry

This article describes a workflow for the analysis of phenolic components in wine enabling confident differential analysis using high performance liquid chromatography (HPLC) in combination with low-field drift-tube ion mobility quadrupole time-of-flight mass spectrometry (IMS-QTOF-MS).


Samantha Duong

Latest:

Measuring Phytosterols in Fortified Food

A balanced diet is one step closer to a healthy lifestyle. Samantha Duong from the Australian Government’s National Measurement Institute (NMI) has used gas chromatography with flame ionization detection (GC–FID) to measure phytosterols in fortified food. She recently spoke to us about this research.


Kenneth C. Parker

Latest:

Quantitation of Albumin and Creatinine in Urine by MALDI-TOF Mass Spectrometry

This MS-based method represents a simple, fast, and attractive alternative to current immunoassay-based methods for the quantitation of albumin and creatinine in urine. This protocol enables the direct detection and measurement of the intact analytes from the same sample preparation, requiring only a 10-fold dilution of a urine sample into a MALDI-TOF matrix solution.


Marvin L. Vestal

Latest:

Quantitation of Albumin and Creatinine in Urine by MALDI-TOF Mass Spectrometry

This MS-based method represents a simple, fast, and attractive alternative to current immunoassay-based methods for the quantitation of albumin and creatinine in urine. This protocol enables the direct detection and measurement of the intact analytes from the same sample preparation, requiring only a 10-fold dilution of a urine sample into a MALDI-TOF matrix solution.


David A. Herold

Latest:

Quantitation of Albumin and Creatinine in Urine by MALDI-TOF Mass Spectrometry

This MS-based method represents a simple, fast, and attractive alternative to current immunoassay-based methods for the quantitation of albumin and creatinine in urine. This protocol enables the direct detection and measurement of the intact analytes from the same sample preparation, requiring only a 10-fold dilution of a urine sample into a MALDI-TOF matrix solution.


Stephen J. Hattan

Latest:

Quantitation of Albumin and Creatinine in Urine by MALDI-TOF Mass Spectrometry

This MS-based method represents a simple, fast, and attractive alternative to current immunoassay-based methods for the quantitation of albumin and creatinine in urine. This protocol enables the direct detection and measurement of the intact analytes from the same sample preparation, requiring only a 10-fold dilution of a urine sample into a MALDI-TOF matrix solution.


Jane Y. Yang

Latest:

Quantitation of Albumin and Creatinine in Urine by MALDI-TOF Mass Spectrometry

This MS-based method represents a simple, fast, and attractive alternative to current immunoassay-based methods for the quantitation of albumin and creatinine in urine. This protocol enables the direct detection and measurement of the intact analytes from the same sample preparation, requiring only a 10-fold dilution of a urine sample into a MALDI-TOF matrix solution.


Lucie Nováková

Latest:

Advances in Sample Preparation for Biological Fluids

Sample preparation techniques in bioanalysis are multistep, time-consuming, and labour-intensive procedures that can take up 60–80% of the total analysis time. Sample preparation is often the limiting step of fast bioanalysis and the most error-prone part of the analytical method. There is currently a focus on improving the sample preparation process by shortening sample preparation time, cutting the cost of analysis, decreasing sample volume and solvent consumption, reducing the number of sample preparation steps, and adapting the whole process for automation. This article explores microextraction techniques, selective approaches, on-line sample preparation, and dried matrix spots that aim to provide solutions to sample preparation problems in bioanalysis.


Karen Gaudin

Latest:

Quality by Design: A Tool for Separation Method Development in Pharmaceutical Laboratories

Quality by design (QbD) has gained in importance in the pharmaceutical industry and is supported by several regulatory documents (ICH, FDA). The aim is to ensure product quality through a better understanding of products and processes during pharmaceutical development. As analytical procedures are critical processes of pharmaceutical product development and quality control (QC), QbD has become a key tool in the development of analytical methods. This article outlines the general trends observed when applying QbD to the development of separation methods in pharmaceutical analysis. The main pharmaceutical applications are reviewed along with a detailed description of tools involved in QbD methodology. A focus on QbD benefits for the pharmaceutical industry is provided.


Ludivine Ferey

Latest:

Quality by Design: A Tool for Separation Method Development in Pharmaceutical Laboratories

Quality by design (QbD) has gained in importance in the pharmaceutical industry and is supported by several regulatory documents (ICH, FDA). The aim is to ensure product quality through a better understanding of products and processes during pharmaceutical development. As analytical procedures are critical processes of pharmaceutical product development and quality control (QC), QbD has become a key tool in the development of analytical methods. This article outlines the general trends observed when applying QbD to the development of separation methods in pharmaceutical analysis. The main pharmaceutical applications are reviewed along with a detailed description of tools involved in QbD methodology. A focus on QbD benefits for the pharmaceutical industry is provided.



Ronald de Vries

Latest:

High-Throughput Analysis of Drugs and Metabolites in Biological Fluids Using Quan–Qual Approaches

The new generation of high-resolution mass spectrometry (HRMS) systems offers high sensitivity, dynamic range, resolution, accuracy, and scan-to-scan reproducibility, enabling high-throughput quantitative analyses in combination with information-rich qualitative data. The most recently released HRMS systems offer an alternative to triple quadrupole (TQ)-MS systems. This provides a huge opportunity to obtain quantitative and qualitative information from one analysis, but also requires a different mindset and expertise to make the right choices and compromises to get the most information from your sample.


Julie Schappler

Latest:

Characterization of Counterfeit and Substandard Medicines Using Capillary Electrophoresis

The proportion of counterfeit medicines has increased dramatically. Combatting this issue is complex, and various levels of action are necessary. The quality control (QC) of imported batches using simple, reliable, and cost-efficient analytical approaches is vital. Capillary electrophoresis (CE) is becoming important because the analysis is achieved in a capillary with small dimensions, and is usually filled with an aqueous buffer. No organic solvent is required and injection volumes are in the nanolitre range, which is convenient because of the low availability of reference substances and reduces the environmental impact. CE is now recognized by numerous Pharmacopeia and can be used for counterfeit and substandard characterization as a validated analytical procedure that adheres to international guidelines.


Serge Rudaz

Latest:

Characterization of Counterfeit and Substandard Medicines Using Capillary Electrophoresis

The proportion of counterfeit medicines has increased dramatically. Combatting this issue is complex, and various levels of action are necessary. The quality control (QC) of imported batches using simple, reliable, and cost-efficient analytical approaches is vital. Capillary electrophoresis (CE) is becoming important because the analysis is achieved in a capillary with small dimensions, and is usually filled with an aqueous buffer. No organic solvent is required and injection volumes are in the nanolitre range, which is convenient because of the low availability of reference substances and reduces the environmental impact. CE is now recognized by numerous Pharmacopeia and can be used for counterfeit and substandard characterization as a validated analytical procedure that adheres to international guidelines.


Quantum Analytics

Latest:

Breaking Down the Microplastics Problem with Pyrolysis-GC/MS

Professor Wan-Tang (Grace) Chen of the University of Massachusetts Lowell accepted our invite to participate in a virtual Q&A session. Dr. Chen directs the Plastics & Environment Research Laboratory at the university and was gracious enough to share what her team is working on, and how they’re leveraging the Pyrolysis-GC/MS technique in novel microplastics research.


Lipika Basumallick

Latest:

Glycoprotein Monosaccharide Analysis Using HPAE-PAD with Eluent Generation

Glycoprotein monosaccharide compositional analysis is important for the development and manufacture of glycoprotein human therapeutics. Here we report a robust method for this analysis. This chromatographic method requires no mobile phase preparation thus saving time and delivering excellent retention time reproducibility that results in good method reproducibility.


Metrohm

Latest:

Fast Edible Oil Composition Analysis with Raman Spectroscopy

This paper demonstrates a fast, non-destructive method for analyzing edible oil composition using Raman spectroscopy, offering an efficient alternative for the lab.






Roger Inloes

Latest:

Ghost Peak Investigation in a Reversed-Phase Gradient LC System

Here is a step-by-step approach to investigate the source of ghost peaks in a gradient LC method.


Daniel L. Shollenberger

Latest:

Evaluation of Retention and Selectivity Using Biphenyl Stationary Phases

In reversed-phase liquid chromatography (LC), C18 alkyl-based stationary phases have been the favourite of method developers. Phenyl stationary phases are an alternative that are thought to benefit from additional π-π mechanisms. Recently, there has been a growing interest in the use of phases based on the biphenyl moiety. This instalment of “Column Watch” looks at the retention mechanisms of biphenyl phases and contrasts them with those of more-common alkyl phases.