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A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (31 July 2020) | Viewed by 25438

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Prof. Dr. Piotr Konieczka

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Department of Analytical Chemistry, Faculty of Chemistry, Gdańsk University of Technology, Gdańsk, Poland
Interests: environmental analysis and monitoring; trace analysis; quality assurance and quality control; chemical metrology; chemical statistics

Special Issue Information

Dear Colleagues,

The main developmental trends in chemical analytics have involved the determination of analytes at ever decreasing detection levels in samples with increasingly complex matrices. This is an extremely difficult and complicated task and, therefore, it poses a great challenge to analytical chemists.

Environmental analytical chemistry is a field of science that draws on experience from many of the sciences (chemistry, biology, physics, and mathematics) to accomplish the primary goal – obtaining reliable information about the investigated objects. Development trends of environmental analytical chemistry can be divided into two basic groups:

Methodological – such as speciation analysis, application of the procedures for the simultaneous determination of multiple analytes, use of summary indicators of assessment of the quality of the environment, the use of biosensors, modification and simplification of the sample preparation step, increasing selectivity of analytical procedures, and the application of green analytical techniques
Instrumental – use of hyphenated techniques, miniaturization, automation, computerization, using new sensors, biosensors, utilization of on-line, in-line, in-situ measurements, and the application of statistical tools and chemometrics for data treatment.

This Special Issue will cover a wide range of topics related to both of groups of trends in environmental analytical chemistry.

Prof. Piotr Konieczka
Guest Editor

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Keywords

method development
method validation
bioanalysis
hyphenated techniques
miniaturization
sensors
biosensors
green analytical chemistry
speciation
monitoring

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Published Papers (6 papers)

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Research

27 pages, 1939 KiB

Open AccessArticle

Risk of Mercury Ingestion from Canned Fish in Poland

by Aleksandra Pawlaczyk, Anna Przerywacz, Magdalena Gajek and Malgorzata Iwona Szynkowska-Jozwik

Molecules 2020, 25(24), 5884; https://doi.org/10.3390/molecules25245884 - 12 Dec 2020

Cited by 7 | Viewed by 5009

Abstract

In this study, total mercury content was determined in 84 canned fish corresponding to commonly consumed brands (over 14 different producers), which were purchased from local markets in Poland in the years 2019–2020. For comparison purposes, samples of both the matrix in which the fish were kept along with the seafood samples were measured. The analyses were carried out using the cold vapor AAS technique. Statistical analyses were employed to identify significant differences in mercury content in relation to the selected criteria such as fish species, type of fish (predatory, non-predatory) and the producer brand. The obtained results were compared against domestic and international standards as well as with the literature data in order to evaluate the safety of the canned fish consumption. The study revealed that none of canned fish exceeded the acceptable levels set by the FAO/WHO. The highest amount of Hg was recorded for canned tuna (maximum 351.30 µg/kg, mean 74.38 µg/kg). Further, the estimated tolerable dose of weekly mercury intake suggests that the consumption of over 1.8 cans of fish with the highest mean mercury content should not pose a risk to consumers in Poland according to international standards. Among the ten highest mean results for mercury, five of them belonged to canned tuna (Bonito species) kept in different matrices. These consisted of seven domestic and three imported brands of fish products, which is a worrying message for a local community. Mercury content in predatory fish differed significantly from the results gathered for non-predatory fish and the total amount of mercury in studied canned fish corresponded to their status in the aquatic food chain. Moreover, significant differences were stated between various fish species and fishing areas. Fish caught in the Atlantic Ocean (cod and herring) presented higher mercury content than the ones from closed seas. Full article

(This article belongs to the Special Issue Trends in Environmental Analytical Chemistry)

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11 pages, 1091 KiB

Open AccessCommunication

Evaluation of a Stable Isotope-Based Direct Quantification Method for Dicamba Analysis from Air and Water Using Single-Quadrupole LC–MS

by Manoj Ghaste, Nicholas C. Hayden, Matthew J. Osterholt, Julie Young, Bryan Young and Joshua R. Widhalm

Molecules 2020, 25(16), 3649; https://doi.org/10.3390/molecules25163649 - 11 Aug 2020

Cited by 10 | Viewed by 3374

Abstract

Dicamba is a moderately volatile herbicide used for post-emergent control of broadleaf weeds in corn, soybean, and a number of other crops. With increased use of dicamba due to the release of dicamba-resistant cotton and soybean varieties, growing controversy over the effects of spray drift and volatilization on non-target crops has increased the need for quantifying dicamba collected from water and air sampling. Therefore, this study was designed to evaluate stable isotope-based direct quantification of dicamba from air and water samples using single-quadrupole liquid chromatography–mass spectrometry (LC–MS). The sample preparation protocols developed in this study utilize a simple solid-phase extraction (SPE) protocol for water samples and a single-step concentration protocol for air samples. The LC–MS detection method achieves sensitive detection of dicamba based on selected ion monitoring (SIM) of precursor and fragment ions and relies on the use of an isotopically labeled internal standard (IS) (D₃-dicamba), which allows for calculating recoveries and quantification using a relative response factor (RRF). Analyte recoveries of 106–128% from water and 88–124% from air were attained, with limits of detection (LODs) of 0.1 ng mL⁻¹ and 1 ng mL⁻¹, respectively. The LC–MS detection method does not require sample pretreatment such as ion-pairing or derivatization to achieve sensitivity. Moreover, this study reveals matrix effects associated with sorbent resin used in air sample collection and demonstrates how the use of an isotopically labeled IS with RRF-based analysis can account for ion suppression. The LC–MS method is easily transferrable and offers a robust alternative to methods relying on more expensive tandem LC–MS/MS-based options. Full article

(This article belongs to the Special Issue Trends in Environmental Analytical Chemistry)

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17 pages, 3452 KiB

Open AccessArticle

Method Validation and Investigation of the Levels of Pharmaceuticals and Personal Care Products in Sludge of Wastewater Treatment Plants and Soils of Irrigated Golf Course

by Olufemi Temitope Ademoyegun, Omobola Oluranti Okoh and Anthony Ifeanyi Okoh

Molecules 2020, 25(14), 3114; https://doi.org/10.3390/molecules25143114 - 8 Jul 2020

Cited by 15 | Viewed by 2928

Abstract

The validation of a sensitive and reliable analytical procedure for the determination of pharmaceutical and personal care products (PPCPs) in solid environmental samples is reported in this study. Initially, two types of derivatization were used for the identification of the 13 target PPCP standards (acylation and silylation), but silylation proved to be better in sensitivity as it detected all of the analytes under investigation. Samples were extracted using an ultrasonicator, concentrated and re-dissolved in 100 mL water, then cleaned-up using C18 cartridges before silylation that preceded the Gas chromatography-mass Spectrometry detector (GC–MS) analyses. The optimized method provided a linear response over the range of 10–400 ng·g⁻¹ with r² > 0.992 and satisfactory recoveries (>45.6%) for the 13 compounds of interest. In this study, the variation of the sonication temperature, type of organic solvent for extraction, and types of cartridge were used to optimize the extraction procedure. A good repeatability (within day) and reproducibility (between days) with a relative standard deviation (RSD) that was equal or less than 13% for all the PPCPs were achieved with the developed extraction procedures for the irrigated soil and sewage sludge samples. The limits of detection (LODs) of the tested compounds varied from 0.1 ng·g⁻¹ (aspirin) to 1.4 ng·g⁻¹ (doxycycline) and from 0.1 ng·g⁻¹ (codiene) to 1.7 ng·g⁻¹ (doxycycline) for soils and sewage sludge samples, respectively. The method was successfully applied to the sludge of wastewater treatment plants and soils of an irrigated golf course. Among the tested emerging pollutants, paracetamol showed the highest concentration value of 98.9 ng·g⁻¹ in the sludge, and for the irrigated soil (0 to 10 cm), the concentration ranged from 1.16 ng·g⁻¹ (aspirin) to 8.57 ng·g⁻¹ (ibuprofen). Full article

(This article belongs to the Special Issue Trends in Environmental Analytical Chemistry)

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10 pages, 563 KiB

Open AccessArticle

Optimization of QuEChERS Method for Simultaneous Determination of Neonicotinoid Residues in Pollinator Forage

by Maura J. Hall, Viet Dang, Steven P. Bradbury and Joel R. Coats

Molecules 2020, 25(12), 2732; https://doi.org/10.3390/molecules25122732 - 12 Jun 2020

Cited by 11 | Viewed by 4300

Abstract

Consistent with the large-scale use of pesticide seed treatments in U.S. field crop production, there has been an increased use of neonicotinoid-treated corn and soybean seed over the past decade. Neonicotinoids can move downwind to adjacent off-field pollinator habitats in dust from planting and/or move downslope to habitats in surface water. The extent of potential neonicotinoid exposure to pollinators from neonicotinoid movement into these adjacent pollinator habitats is unclear. Pollen and leaf tissue extractions were completed using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction procedure. Samples were subjected to a clean-up step using dispersive solid-phase extraction (dSPE) techniques prior to analysis. The compounds in the extracts were separated on a reversed-phase column with gradient elution and confirmed with tandem mass spectrometry. The extraction method showed acceptable recoveries of analytes ranging from 78.4 to 93.6% and 89.4 to 101% for leaf tissue and pollen, respectively. The method’s detection limits ranged from 0.04 to 0.3 ng/g in milkweed leaf tissue and 0.04 to 1.0 ng/g in pollen. The method is currently being employed in ongoing studies surveying pollen from a diversity of forbs and milkweed leaves obtained from habitat patches established within fields with a history of using neonicotinoid-treated seeds. Full article

(This article belongs to the Special Issue Trends in Environmental Analytical Chemistry)

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20 pages, 2277 KiB

Open AccessFeature PaperArticle

Organic Acids and Polyphenols Determination in Polish Wines by Ultrasound-Assisted Solvent Extraction of Porous Membrane-Packed Liquid Samples

by Alicia D. Robles, Magdalena Fabjanowicz, Justyna Płotka-Wasylka and Piotr Konieczka

Molecules 2019, 24(23), 4376; https://doi.org/10.3390/molecules24234376 - 29 Nov 2019

Cited by 27 | Viewed by 4392

Abstract

In the near future, Poland is going to have more and more favorable conditions for viticulture. Organic acids and polyphenols are among the most commonly analyzed compounds due to their beneficial properties for human health and their importance in the winemaking process. In this work, a new technique involving ultrasound-assisted solvent extraction of porous membrane-packed liquid samples (UASE-PMLS) was for the first time described and applied for real samples. The methodology based on UASE-PMLS for organic acids and polyphenols in wine samples was optimized and validated. Using the new technique coupled to GC–MS, organic acids and polyphenols were evaluated in Polish wine samples. Extraction solvent, extraction temperature, derivatization time and sample pH were optimized. Chemometric tools were used for data treatment. Good linearity was obtained for the concentration ranges evaluated with r values between 0.9852 and 0.9993. All parameters of method validation (intra- and inter-day precision and matrix effect) were over 80% with coefficient of variation (CV) up to 17%. Recovery was between (92.0 ± 8.5)% and (113 ± 16)%. Finally, green assessment was evaluated using Analytical Eco-Scale and Green Analytical Procedure Index (GAPI). The UASE-PMLS is characterized by many advantages, e.g., the extraction process is fast and easy coupled to GC–MS. Regarding other extraction techniques, the amount of used solvent is minimum, and no waste is generated. Therefore, it is an environmentally friendly technique. Full article

(This article belongs to the Special Issue Trends in Environmental Analytical Chemistry)

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16 pages, 1248 KiB

Open AccessArticle

Speciation of Chromium in Alkaline Soil Extracts by an Ion-Pair Reversed Phase HPLC-ICP MS Method

by Barbara Leśniewska and Beata Godlewska-Żyłkiewicz

Molecules 2019, 24(6), 1172; https://doi.org/10.3390/molecules24061172 - 25 Mar 2019

Cited by 16 | Viewed by 4235

Abstract

The aim of this work was to study by a hyphenated HPLC-ICP MS technique the chromium species released during alkaline extraction of various soils collected from a contaminated area of an old tannery. An ultrasound-assisted extraction procedure using 0.1 mol L⁻¹ Na₂CO₃ solution was developed for the release of chromium species from the soil. The chromium species in the soil extracts were separated on a C₈ column using EDTA and TBAH solution as a mobile phase. The use of an ICP-QQQ MS spectrometer in tandem mass configuration (MS/MS) combined with an octopole reaction system (ORS³) pressurized with helium allows one to eliminate spectral interferences during Cr determination in the soil extracts. The detection limit of the procedure was 0.08 µg L⁻¹ for Cr(III) and 0.09 µg L⁻¹ for Cr(VI) species. The trueness of the IP RP HPLC-ICP MS method was proved by an analysis of CRM 041 and CRM 060. The advantage of the proposed method is the analysis of soil extracts without their preliminary neutralization, which limits the losses of Cr(VI) due to the reduction process. The analysed soils mainly contained chromium in immobile forms (94.6–98.5% of the total Cr content). In all alkaline soil extracts mostly the Cr(VI) form was found, but in the extract of organic soils Cr(III) was also present. This arose from the reduction of Cr(VI) species by organic matter (humic acids) and Fe(II). The amount of formed Cr(III) species was dependent on the type of soil (content of organic matter, Mn and Fe) and its moistness. For the first time, the presence of neutral and non-polar chromium fractions in the soil extracts was also demonstrated. It was found that reliable speciation analysis results could be obtained for mineral soils. Full article

(This article belongs to the Special Issue Trends in Environmental Analytical Chemistry)

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