Environmental Analysis

Per- and polyfuorinated alkyl substances (PFAS) are a rapidly growing environmental and human health concern. Owing to their broad commercial use, chemical stability, and bioaccumulation potential, these compounds are widely dispersed in the environment and can cause exposure through many potential pathways. To adequately estimate exposure risks, analytical methods are required that can measure low levels of PFAS compounds in many types of matrices. As will be described, recent advances in solid-phase extraction (SPE) and liquid chromatography tandem mass spectrometry (LC–MS/MS) have enabled the identification and quantification of a large number of PFAS compounds at low concentration (

LCGC Europe spoke to Andrew Turner, Principal Chemist in the Food Safety Group at the Centre for Environment, Fisheries, and Aquaculture Science (Cefas) in Weymouth, UK, about developing a simple ultrahigh-pressure liquid chromatography tandem mass spectrometry (UHPLCÐMS/MS) method for the quantitation of microcystins and nodularin in various sample matrices.

James Stry of FMC Agricultural Solutions talks about best practices for developing robust environmental analysis methods, including simplifying sample preparation and dealing with matrix effects.

The chemical analysis of organic compounds in environmental samples is often targeted on predetermined analytes. A major shortcoming of this approach is that it invariably excludes a vast number of compounds of unknown relevance. Nontargeted chemical fingerprinting analysis addresses this problem by including all compounds that generate a relevant signal from a specific analytical platform and so more information about the samples can be obtained. A DHS−TD−GC−MS method for the fingerprinting analysis of mobile VOCs in soil is described and tested in this article. The analysis parameters, sorbent tube, purge volume, trapping temperature, drying of sorbent tube, and oven temperature were optimized through qualitative and semiquantitative analysis. The DHS−TD–GC−MS fingerprints of soil samples from three sites with spruce, oak, or beech were investigated by pixel-based analysis, a nontargeted data analysis method.

Mira Petrovic from the Catalan Institute for Water Research (ICRA) in Girona, Spain, reveals the advantages and practical applications of a novel method she developed for the multiresidue trace analysis of pharmaceutical compounds and their corresponding metabolites and transformation products using dual-column liquid chromatography (LC) coupled to tandem mass spectrometry (MS/MS).

Mira Petrovic from the Catalan Institute for Water Research (ICRA) in Girona, Spain, reveals the advantages and practical applications of a novel method she developed for the multiresidue trace analysis of pharmaceutical compounds and their corresponding metabolites and transformation products using dual-column liquid chromatography (LC) coupled to tandem mass spectrometry (MS/MS).

In the environmental analytical chemistry literature, the topic of matrix interferences and matrix effects has not been addressed in a fundamental way. Here, we examine which methods appear to have a tendency for matrix interference and suggest ways to reduce the problem.

As part of the Earth Day celebration in Dallas, Texas, USA, earlier this year, the Collaborative Laboratories for Environmental Analysis and Remediation (CLEAR) at U.T. Arlington hosted the first annual Responsible Shale Energy Extraction (RSEE) symposium. Even though Kevin Schug and his group have been very involved in this conversation for the past several years, several points stood out.

Monitoring the endocrine status of marine mammals can give valuable information to researchers. Overall health, health issues, and an animal’s pregnancy status can all be deduced from the careful analysis of steroid hormones. However, gaining such data is not easy. The difficulty of obtaining blood samples in the wild necessitates the use of alternative matrices, such as blubber, that in turn provide a number of analytical challenges. Aiming to solve these issues a team of researchers from the National Institute of Standards and Technology (NIST) have developed a novel method using liquid chromatography tandem mass spectrometry (LC–MS/MS) to analyze blubber obtained through remote sample collection. Ashley Boggs from NIST spoke to The Column about the benefits of this newly developed technique and its potential wider application in animal research and management.

This study describes the gas chromatography–mass spectrometry (GC–MS) analysis of trace-level “air toxics” in humidified cannister air, using cryogen-free preconcentration technology. We show that this method is able to detect 65 target compounds ranging from propene to naphthalene, with method detection limits as low as 0.7 pptv in SIM mode, making it compliant both with standard TO-15 methods, and with “trace TO-15” methods stipulating lower detection limits.

You don’t have to look far to find headlines such as “PFAS Chemicals in Drinking Water Prompts Restrictions” (1) or “Toxic Algae Discovered in Waterways off Lake Tahoe” (2). These two examples highlight key environmental concerns, and laboratories are feeling the demands to perform more of these tests. The first headline relates to the pollution from per- and polyfluorinated alkyl substances (PFASs) and the latter is attributed to the problems of microcystins and nodularins in water. This article will look into analytical workflows that can be applied to the testing of these “in demand” compounds.

This article evaluates ASTM D7979-16 for the “direct” analysis of 30 PFCs and 19 mass-labeled surrogates. Instead of using solid-phase extraction, the PFCs were solubilized in a methanol–water mix and filtered if necessary, and the sample was injected into a LC–MS/MS system.

The Royal Society of Chemistry’s Environmental Chemistry Group, Water Science Forum, and the Separation Science Group Joint Meeting was held on Friday 3 March 2017 at the Science Suite of the Royal Society of Chemistry, in Burlington House, Piccadilly, London, UK.

Environmental analyses of food, soil, and water have changed dramatically over the last decade. Topics such as pesticides, food additives, and natural products have become important as food products are globally grown and distributed (1). Monitoring their quality is critical to international business. Pharmaceuticals, fluorinated surfactants, and endocrine disruptors in water are major new topics, where not only parent compounds are unknown but also their metabolites and degradation products are often more important or more abundant than the parent compound (2). New environmental issues, such as hydraulic fracturing and its wastewater, have captured our attention as the production of oil and gas has increased exponentially in the past decade (3). With this technology comes the problem of wastewater disposal and groundwater contamination. These environmental issues have greatly benefited from the combination of ultrahigh‑performance liquid chromatography (UHPLC) mated to high resolution mass spectrometry (HRMS

How to improve results by optimizing the injection, column, and detection.

This article will focus on the development of an optimized gas chromatography–mass spectrometry (GC–MS) method that improves upon the current EPA and European detection limit requirements for BTEX compounds and meets all other criteria described in EPA Method 524.2 for the measurement of purgeable organic compounds in water by capillary column GC–MS.

The occurrence of disinfection byproducts in natural waters poses a health risk for humans as well as aquatic organisms. This article presents a method, which was recently developed at the University of Arizona, in Tucson, Arizona, USA, for the fast and simultaneous determination of 15 regulated and unregulated disinfection byproducts.

This is the first in a series of articles exploring current topics in separation science that will be addressed at the HPLC 2017 conference in Prague, Czech Republic, from 18–22 June.

Improve results by optimizing the injection, column, and detection.

Electrophoretic concentration (EC) is an electric field-driven and environmentally friendly off-line sample preparation for charged analytes. EC was demonstrated for the enrichment of either six anionic pollutants or five cationic drugs from purified, drinking, river, or waste- water samples. EC provided analyte enrichment in 15–50 min with concentration factors of 30–249 and 12–243 for the negatively and positively charged analytes, respectively. A modification of the EC device enabled simultaneous EC and separation (SECS) of six cationic and anionic herbicides with concentration factors of 18–337 in 30 min. The potential of SECS has also been evaluated for the determination of high mobility ions in urine and the results obtained have been compared to common acetonitrile treatment of urine. SECS provided an enrichment of high mobility ions and revealed more peaks compared to the acetonitrile treatment.

The Royal Society of Chemistry’s Environmental Chemistry Group, Water Science Forum, and the Separation Science Group Joint Meeting will be held on Friday 3 March 2017 at the Science Suite of the Royal Society of Chemistry, in Burlington House, Piccadilly, London, UK.

Evan Palmer-Young of the University of Massachusetts at Amherst, Amherst, Massachusetts, USA, and Philip Stevenson of the Royal Botanic Gardens, Kew, London, UK, spoke to The Column about their work on bumblebee resistance to the trypanosome parasite Crithidia bombi and the role of chromatography in this research.

Australia’s Great Barrier Reef (GBR) stretches over 2300 km and is composed of over 3000 individual reef systems. The health of the reef therefore often comes under international scrutiny. Hilton Swan from Southern Cross University in Australia has been investigating volatile organic compound (VOC) emissions from the Great Barrier Reef using gas chromatography–mass spectrometry (GC–MS). He recently spoke to The Column about this work.

The Royal Society of Chemistry’s Environmental Chemistry Group, Water Science Forum, and the Separation Science Group Joint Meeting will be held on Friday 3 March 2017 at the Science Suite of the Royal Society of Chemistry, in Burlington House, Piccadilly, London, UK.