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Advances in Analytical Sample Preparation Using Sorbent/Solid Phase Materials as Extraction Media

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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 (28 February 2023) | Viewed by 18781

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Special Issue Editors

Dr. Paraskevas D. Tzanavaras

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Guest Editor

Laboratory of Analytical Chemistry, School of Chemistry, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
Interests: automation; sequential injection analysis; separation techniques (HPLC, CE); post-column derivatization; microextraction
Special Issues, Collections and Topics in MDPI journals

Dr. Constantinos K. Zacharis

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Guest Editor

Laboratory of Pharmaceutical Analysis, Department of Pharmaceutical Technology, School of Pharmacy, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
Interests: pharmaceutical analytical chemistry; method development and validation; sample preparation (derivatization, microextraction, etc.); liquid and gas chromatography; capillary electrophoresis; mass spectrometry
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Despite the huge advancements in chemical instrumentation, sample preparation is always considered as one of the most critical—and in many cases inevitable—steps during chemical analysis. In many cases, pitfalls in analytical results are associated with sample preparation, including loss of analytes, insufficient extraction, conversion of compounds to undetectable species, etc.

Trends in sample preparation are moving towards the development of faster, greener, and automated approaches, mostly taking advantage of progresses in material science. Of course, selectivity and efficiency should always be the primary targets. Sample preparation based on sorbent/solid phase extraction protocols (SPE, SPME, QuEChERS, SBSE, etc.) seem to be most promising to fulfil the above requirements, and tend to dominate traditional liquid extraction analogous schemes.

The present Special Issue aims to cover the latest research trends and applications of sample preparation based on sorbent/solid phase extraction strategies. Researchers working on all aspects of basic research and applications in food, environmental, and biomedical sciences are cordially invited to contribute a research or review article to this Special Issue. Representative topics include (but are certainly not limited to): solid phase extraction (SPE), solid phase microextraction (SPME), automated extraction schemes, new materials, QuEChERS, fabric sorptive-based extractions, etc.

Dr. Constantinos K. Zacharis
Dr. Paraskevas D. Tzanavaras
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Molecules is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

solid phase extraction (SPE)
solid phase microextraction (SPME)
matrix solid phase dispersion (MSPD)
QuEChERS
fabric sorptive phase extraction (FPSE)
automation
new materials/sorbents (MOF, COFs, nanomaterials, conductive polymers, magnetic materials, etc.)
sample preparation
green analytical chemistry
miniaturization in sample preparation
stir bar sorptive extraction (SBSE)
capsule phase microextraction

Published Papers (8 papers)

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Research

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15 pages, 2307 KiB

Open AccessArticle

Pollution, Exposure and Risk of Biogenic Amines in Canned Sea Fish: Classification of Analytical Methods Based on Carbon Spheres QuEChERS Extraction Combined with HPLC

by Xinying Guo, Zhiying Dai and Weibing Zhang

Molecules 2022, 27(19), 6243; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27196243 - 22 Sep 2022

Cited by 2 | Viewed by 1305

Abstract

This study investigated the pollution characteristics, exposure levels and health risk assessments of seven kinds of biogenic amines (BAs) in eight varieties of canned sea fish products (n = 131) on the Chinese market. Carbon spheres QuEChERS mixed dispersion solid phase extraction combined with HPLC was used for the classification and analysis of batch samples. The average recovery of single BAs obtained by this method is 92.3~97.7%, and the relative standard deviation is 1.9~4.8%. Different varieties of samples have different degrees of pollution, the mass concentration of single BAs range 0.45~27.74 mg/kg, and the total concentration of ΣBAs range 18.77~368.50 mg/kg, of which the concentration of Σ4BAs range 11.53~368.50 mg/kg. The composition of four BAs is mainly putrescine, cadaverine, histamine and tyramine, which always play an important role in the exposure level and risk assessment of samples. The exposure level of BAs in the human body ranges 67.03~209.52 μg∙kg⁻¹∙d⁻¹. The health risk assessment shows that the gender trend of exposure risk level of BAs is male > female (young age), female > male (middle and old age), the age trend is young age > old age > middle age, and the regional trend is city > countryside. The food safety index of BAs in samples is 0.0062~0.0195, which is far less than 1, so the risk is within the controllable range. Full article

(This article belongs to the Special Issue Advances in Analytical Sample Preparation Using Sorbent/Solid Phase Materials as Extraction Media)

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13 pages, 2550 KiB

Open AccessArticle

Magnetic Torus Microreactor as a Novel Device for Sample Treatment via Solid-Phase Microextraction Coupled to Graphite Furnace Atomic Absorption Spectroscopy: A Route for Arsenic Pre-Concentration

by Sofía Ortegón, Paula Andrea Peñaranda, Cristian F. Rodríguez, Mabel Juliana Noguera, Sergio Leonardo Florez, Juan C. Cruz, Ricardo E. Rivas and Johann F. Osma

Molecules 2022, 27(19), 6198; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27196198 - 21 Sep 2022

Cited by 3 | Viewed by 1625

Abstract

This work studied the feasibility of using a novel microreactor based on torus geometry to carry out a sample pretreatment before its analysis by graphite furnace atomic absorption. The miniaturized retention of total arsenic was performed on the surface of a magnetic sorbent material consisting of 6 mg of magnetite (Fe₃O₄) confined in a very small space inside (20.1 µL) a polyacrylate device filling an internal lumen (inside space). Using this geometric design, a simulation theoretical study demonstrated a notable improvement in the analyte adsorption process on the solid extractant surface. Compared to single-layer geometries, the torus microreactor geometry brought on flow turbulence within the liquid along the curvatures inside the device channels, improving the efficiency of analyte–extractant contact and therefore leading to a high preconcentration factor. According to this design, the magnetic solid phase was held internally as a surface bed with the use of an 8 mm-diameter cylindric neodymium magnet, allowing the pass of a fixed volume of an arsenic aqueous standard solution. A preconcentration factor of up to 60 was found to reduce the typical “characteristic mass” (as sensitivity parameter) determined by direct measurement from 53.66 pg to 0.88 pg, showing an essential improvement in the arsenic signal sensitivity by absorption atomic spectrometry. This methodology emulates a miniaturized micro-solid-phase extraction system for flow-through water pretreatment samples in chemical analysis before coupling to techniques that employ reduced sample volumes, such as graphite furnace atomic absorption spectroscopy. Full article

(This article belongs to the Special Issue Advances in Analytical Sample Preparation Using Sorbent/Solid Phase Materials as Extraction Media)

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13 pages, 1696 KiB

Open AccessArticle

A Strategy for Sample Preparation: Using Egg White Gel to Promote the Determination of Aflatoxin M1 Content in Milk Samples

by Xiao Ning, Lulu Wang, Shaoming Jin, Xuran Fu, Xiulan Sun and Jin Cao

Molecules 2022, 27(15), 5039; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27155039 - 08 Aug 2022

Cited by 2 | Viewed by 1446

Abstract

The analysis of food samples is a challenging task. The high complexity of food matrices hinders the extraction and detection of analytes from them. Therefore, the correct preparation of food samples is a crucial step for their subsequent analysis, as it achieves the proper isolation and preconcentration of analytes and removes the interfering proportion of the food matrix before instrumental analysis. We aimed to develop a method that not only satisfies the requirement of detecting trace compounds in complex matrices but also achieves a “greener” approach by reducing the use of organic solvents and non-degradable materials to minimize the health hazards posed to the operators as well as pollution to the environment. In this study, we prepared egg white as a concentrated gel and used this material for the biological purification of milk samples. After the milk protein was removed by acidification and salting, the residual amount of aflatoxin M1 in milk samples was quantitatively determined by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The results showed that the novel egg white purification method possessed advantages over the immunoaffinity technique used as the reference method in extraction recovery, sensitivity, repeatability, and operability. The limit of detection (LOD) was 0.001 μg/kg. In spiked samples containing 0.01 μg/kg to 2 μg/kg of AFM1, the average recovery was 88.3–94.7%, with a precision of 6.1–11.0%. Improved repeatability was obtained by significantly reducing the operation time and resource requirements compared with the immunoaffinity technique currently used internationally. This study provides a reference for the further improvement of the relevant international standards in place for the detection of aflatoxin M1 in milk. Full article

(This article belongs to the Special Issue Advances in Analytical Sample Preparation Using Sorbent/Solid Phase Materials as Extraction Media)

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15 pages, 3008 KiB

Open AccessArticle

Development of a Quantitative Method for Detection of Multiclass Veterinary Drugs in Feed Using Modified QuPPe Extraction and LC–MS/MS

by Sunyeong Jang, Hyungju Seo, Hojin Kim, Hyoyoung Kim, Jongsung Ahn, Hyunjeong Cho, Sunghie Hong, Seunghwa Lee and Taewoong Na

Molecules 2022, 27(14), 4483; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27144483 - 13 Jul 2022

Cited by 8 | Viewed by 2142

Abstract

A method was developed for the rapid and quantitative analysis of 30 veterinary drugs belonging to 17 classes (amphenicols (1), anthelmintics (1), cephalosporins (4), coccidiostats (1), lincosamides (1), macrolide (1), nitroimidazole (1), penicillins (3), phenylhydrazines (1), polypeptides (1), pyrethrins (1), quinolones (5), sulfonamides (3), tetracycline (3), neuroleptic agents (1), triazene trypanocidal agents (1), other. (1)) in feeds. The proposed method with a modified Quick Polar Pesticides (QuPPe) sample preparation was validated for the determination of 30 veterinary drugs in feed samples by liquid chromatography triple-quadrupole mass spectrometry (LC–MS/MS). The sample was extracted with methanol containing 1% acetic acid and purified by dispersive solid-phase extraction (d-SPE) with C18. Good linearity (r² ≥ 0.98) was observed, and the LOQ values ranged from 10 to 200 µg/kg. Average recoveries ranged from 70.8 to 118.4%, and the relative standard deviation was ≤ 18.7%. This validated method was used in the determination of 30 veterinary drugs in 142 feed samples obtained from South Korea. The results show that lincomycin was present in only one of the tested feed samples, although it was detected at a value lower than the LOQ. In conclusion, this multi-residue method can be used for screening through the detection and quantitation of residual multiclass veterinary drugs in feed samples. Full article

(This article belongs to the Special Issue Advances in Analytical Sample Preparation Using Sorbent/Solid Phase Materials as Extraction Media)

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11 pages, 1395 KiB

Open AccessArticle

Packed-Fiber Solid Phase-Extraction Coupled with HPLC-MS/MS for Rapid Determination of Lipid Oxidative Damage Biomarker 8-Iso-Prostaglandin F_2α in Urine

by Ying Sun, Yan Yan and Xuejun Kang

Molecules 2022, 27(14), 4417; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27144417 - 10 Jul 2022

Viewed by 1253

Abstract

The 8-iso-prostaglandin F_2α (8-iso-PGF_2α) biomarker is used as the gold standard for tracing lipid oxidative stress in vivo. The analysis of urinary 8-iso-PGF_2α is challenging when dealing with trace amounts of 8-iso-PGF_2α and the complexity of urine matrixes. A packed-fiber solid-phase extraction (PFSPE)–coupled with HPLC-MS/MS–method, based on polystyrene (PS)-electrospun nanofibers, was developed for the specific determination of 8-iso-PGF_2α in urine and compared with other newly developed LC-MS/MS methods. The method, which simultaneously processed 12 samples within 5 min on a self-made semi-automatic array solid-phase extraction processor, was the first to introduce PS-electrospun nanofibers as an adsorbent for the extraction of 8-iso-PGF_2α and was successfully applied to real urine samples. After optimizing the PFSPE conditions, good linearity in the range of 0.05–5 ng/mL with R² > 0.9996 and a satisfactory limit of detection of 0.015 ng/mL were obtained, with good intraday and interday precision (RSD < 10%) and recoveries of 95.3–103.8%. This feasible method is expected to be used for the batch quantitative analysis of urinary 8-iso-PGF_2α. Full article

(This article belongs to the Special Issue Advances in Analytical Sample Preparation Using Sorbent/Solid Phase Materials as Extraction Media)

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19 pages, 9568 KiB

Open AccessArticle

Molecular Dynamic Study of Mechanism Underlying Nature of Molecular Recognition and the Role of Crosslinker in the Synthesis of Salmeterol-Targeting Molecularly Imprinted Polymer for Analysis of Salmeterol Xinafoate in Biological Fluid

by Shendi Suryana, Mutakin Mutakin, Yudi Rosandi and Aliya Nur Hasanah

Molecules 2022, 27(11), 3619; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27113619 - 05 Jun 2022

Cited by 4 | Viewed by 2099

Abstract

The rational preparation of molecularly imprinted polymers (MIPs) in order to have selective extraction of salmeterol xinafoate (SLX) from serum was studied. SLX is an acting β-adrenergic receptor agonist used in the treatment of asthma and has an athletic performance-enhancing effect. Molecular dynamics were used for the simulation of the SLX-imprinted pre-polymerization system, to determine the stability of the system. The computational simulation showed that SLX as a template, 4-hydroxyethyl methacrylate (HEMA) as a monomer, and trimethylolpropane trimethacrylate (TRIM) as a crosslinker in mol ratio of 1:6:20 had the strongest interaction in terms of the radial distribution functional. To validate the computational result, four polymers were synthesized using the precipitation polymerization method, and MIP with composition and ratio corresponding with the system with the strongest interaction as an MD simulation result showed the best performance, with a recovery of 96.59 ± 2.24% of SLX in spiked serum and 92.25 ± 1.12% when SLX was spiked with another analogue structure. Compared with the standard solid phase extraction sorbent C-18, which had a recovery of 79.11 ± 2.96%, the MIP showed better performance. The harmony between the simulation and experimental results illustrates that the molecular dynamic simulations had a significant role in the study and development of the MIPs for analysis of SLX in biological fluid. Full article

(This article belongs to the Special Issue Advances in Analytical Sample Preparation Using Sorbent/Solid Phase Materials as Extraction Media)

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14 pages, 2794 KiB

Open AccessArticle

Development of a Solid-Phase Extraction Method Based on Biocompatible Starch Polyurethane Polymers for GC-MS Analysis of Polybrominated Diphenyl Ethers in Ambient Water Samples

by Qian Zhang and Chukwunonso P. Okoli

Molecules 2022, 27(10), 3253; https://doi.org/10.3390/molecules27103253 - 19 May 2022

Viewed by 1521

Abstract

A new solid-phase extraction (SPE) method for the extraction, enrichment, and analysis of eight polybrominated diphenyl ethers (PBDEs) in water was developed. The current approach involves using a cross-linked starch-based polymer as an extraction adsorbent and determining the PBDE analytes of interest using gas chromatography-mass spectrometry in negative chemical ionization mode (GC-NCI-MS). The starch-based polymer was synthesized by the reaction of soluble starch with 4,4′-methylene-bis-phenyldiisocyanate as a cross-linking agent in dry dimethylformamide. Various parameters impacting extraction efficiencies, such as adsorbent quantity, sample volumes, elution solvents and volumes, and methanol content, were carefully optimized. The 500 mg of starch-based polymer as an adsorbent used to extract 1000 mL of spiked water, presented high extraction recoveries of eight PBDEs. The linearity of the extraction process was investigated in the range of 1–200 ng L⁻¹ for BDE-28, 47, 99, 100, and 5–200 ng L⁻¹ for BDE-153, 154, 183, and 209, with coefficients of determination (r2) exceeding 0.990 for all PBDEs. The limits of detection (LODs) ranged from 0.06 to 1.42 ng L⁻¹ (S/N = 3) and the relative standard deviation values (RSD) were between 3.6 and 9.5 percent (n = 5) under optimum conditions. The method was successfully used to analyze river and lake water samples, where it exhibited acceptable recovery values of 71.3 to 104.2%. Considering the excellent analytical performance and comparative cost advantage, we recommend the developed starch-based SPE method for routine extraction and analysis of PBDEs in water media. Full article

(This article belongs to the Special Issue Advances in Analytical Sample Preparation Using Sorbent/Solid Phase Materials as Extraction Media)

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Review

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21 pages, 1474 KiB

Open AccessReview

FTIR as a Method for Qualitative Assessment of Solid Samples in Geochemical Research: A Review

by Yana Tkachenko and Przemysław Niedzielski

Molecules 2022, 27(24), 8846; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27248846 - 13 Dec 2022

Cited by 16 | Viewed by 6237

Abstract

This study aims to collect information about soil investigation by FTIR. As we know, the FTIR technique is most often used in organic and bioorganic chemistry, while in geochemistry FTIR spectroscopy is not used very often. Therefore, there is a problem with the identification and interpretation of the IR spectra of minerals contained in sediments and soils. The reason for this is a deficiency of data about characteristic wavenumbers for minerals. Therefore, this study reviews and sums up, in one place, published articles that are connected to an investigation of minerals from 2002 to 2021 (based on the Scopus database). Additionally, the present review highlights various analytical techniques (ATR-FTIR, DRIFT, 2D-IR, and SR-FTIR) and discusses some of them for geochemical study. Additionally, the study describes helpful tools in the data pre-processing of IR spectra (normalization, baseline correction, and spectral derivatives). Full article

(This article belongs to the Special Issue Advances in Analytical Sample Preparation Using Sorbent/Solid Phase Materials as Extraction Media)

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