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Special Issue "Solid Phase Extraction: State of the Art and Future Perspectives"

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

Deadline for manuscript submissions: 30 September 2018

Special Issue Editor

Guest Editor
Prof. Dr. Victoria F. Samanidou

Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece
Website | E-Mail
Interests: analytical chemistry; sample preparation; separations; HPLC; extraction techniques

Special Issue Information

Dear Colleagues,

Beyond any doubt, sample preparation is the most important step prior to sample analysis. It is the step that can guarantee an accurate and rapidly obtained result if applied in a correct manner. Due to the fact that it usually involves more than one step, it is tedious, time consuming, and any potential errors will accumulate and yield an erroneous outcome.

Solid phase extraction (SPE) has been a determinative player in the challenge of chemical analysis during the last decades. In the meantime, many sample preparation approaches have been evolved trying to replace it by promising better and “greener” performance. However, SPE still plays a key role in method development, and advanced sorbent technology can re-orient the traditional approach to new perspectives. This Special Issue aims to review the state of the art of this sample preparation technique and also describe the recent and future advances.

Prof. Dr. Victoria F. Samanidou
Guest Editor

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 papers will be 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 monthly 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 1800 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
  • Microextraction
  • Green Chemistry
  • Sample preparation
  • Preconcentration
  • Clean-up
  • Microextraction by packed syringe
  • Matrix solid phase dispersion
  • Nanomaterials
  • Magnetic solid phase extraction
  • Dispersive solid phase extraction
  • Magnetic sorbents

Published Papers (5 papers)

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Research

Open AccessFeature PaperArticle Carbon Nanohorn Suprastructures on a Paper Support as a Sorptive Phase
Molecules 2018, 23(6), 1252; https://doi.org/10.3390/molecules23061252 (registering DOI)
Received: 3 May 2018 / Revised: 21 May 2018 / Accepted: 22 May 2018 / Published: 24 May 2018
PDF Full-text (1891 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
This article describes a method for the modification of paper with single-wall carbon nanohorns (SWCNHs) to form stable suprastructures. The SWCNHs form stable dahlia-like aggregates in solution that are then self-assembled into superior structures if the solvent is evaporated. Dipping paper sections into
[...] Read more.
This article describes a method for the modification of paper with single-wall carbon nanohorns (SWCNHs) to form stable suprastructures. The SWCNHs form stable dahlia-like aggregates in solution that are then self-assembled into superior structures if the solvent is evaporated. Dipping paper sections into a dispersion of SWCNHs leads to the formation of a thin film that can be used for microextraction purposes. The coated paper can be easily handled with a simple pipette tip, paving the way for disposable extraction units. As a proof of concept, the extraction of antidepressants from urine and their determination by direct infusion mass spectrometry is studied. Limits of detection (LODs) were 10 ng/L for desipramine, amitriptyline, and mianserin, while the precision, expressed as a relative standard deviation, was 7.2%, 7.3%, and 9.8%, respectively. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
Figures

Graphical abstract

Open AccessArticle Preconcentration and Determination of Perfluoroalkyl Substances (PFASs) in Water Samples by Bamboo Charcoal-Based Solid-Phase Extraction Prior to Liquid Chromatography–Tandem Mass Spectrometry
Molecules 2018, 23(4), 902; https://doi.org/10.3390/molecules23040902
Received: 22 March 2018 / Revised: 9 April 2018 / Accepted: 12 April 2018 / Published: 14 April 2018
PDF Full-text (11414 KB) | HTML Full-text | XML Full-text
Abstract
In this work, bamboo charcoal was used as solid-phase extraction adsorbent for the enrichment of six perfluoroalkyl acids (PFAAs) in environmental water samples before liquid chromatography–tandem mass spectrometry analysis. The specific porous structure, high specific surface area, high porosity, and stability of bamboo
[...] Read more.
In this work, bamboo charcoal was used as solid-phase extraction adsorbent for the enrichment of six perfluoroalkyl acids (PFAAs) in environmental water samples before liquid chromatography–tandem mass spectrometry analysis. The specific porous structure, high specific surface area, high porosity, and stability of bamboo charcoal were characterized. Several experimental parameters which considerably affect extraction efficiency were investigated and optimized in detail. The experimental data exhibited low limits of detection (LODs) (0.01–1.15 ng/L), wide linear range (2–3 orders of magnitude and R ≥ 0.993) within the concentration range of 0.1–1000 ng/L, and good repeatability (2.7–5.0%, n = 5 intraday and 4.8–8.3%, n = 5 interday) and reproducibility (5.3–8.0%, n = 3). Bamboo charcoal was successfully used for the enrichment and determination of PFAAs in real environmental water samples. The bamboo charcoal-based solid-phase extraction coupled with liquid chromatography–tandem mass spectrometry analysis possessed great potential in the determination of trace PFAA levels in environmental water samples. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
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Figure 1

Open AccessArticle Efficient Separation of Four Antibacterial Diterpenes from the Roots of Salvia Prattii Using Non-Aqueous Hydrophilic Solid-Phase Extraction Followed by Preparative High-Performance Liquid Chromatography
Molecules 2018, 23(3), 623; https://doi.org/10.3390/molecules23030623
Received: 15 January 2018 / Revised: 7 March 2018 / Accepted: 9 March 2018 / Published: 9 March 2018
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Abstract
An efficient preparative procedure for the separation of four antibacterial diterpenes from a Salvia prattii crude diterpenes-rich sample was developed. Firstly, the XION hydrophilic stationary phase was chosen to separate the antibacterial crude diterpenes-rich sample (18.0 g) into three fractions with a recovery
[...] Read more.
An efficient preparative procedure for the separation of four antibacterial diterpenes from a Salvia prattii crude diterpenes-rich sample was developed. Firstly, the XION hydrophilic stationary phase was chosen to separate the antibacterial crude diterpenes-rich sample (18.0 g) into three fractions with a recovery of 46.1%. Then, the antibacterial fractions I (200 mg), II (200 mg), and III (150 g) were separated by the Megress C18 preparative column, and compounds tanshinone IIA (80.0 mg), salvinolone (62.0 mg), cryptotanshinone (70.0 mg), and ferruginol (68.0 mg) were produced with purities greater than 98%. The procedure achieved large-scale preparation of the four diterpenes with high purity, and it could act as a reference for the efficient preparation of active diterpenes from other plant extracts. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
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Figure 1

Open AccessArticle Sensitive Detection of 8-Nitroguanine in DNA by Chemical Derivatization Coupled with Online Solid-Phase Extraction LC-MS/MS
Molecules 2018, 23(3), 605; https://doi.org/10.3390/molecules23030605
Received: 9 February 2018 / Revised: 4 March 2018 / Accepted: 6 March 2018 / Published: 8 March 2018
Cited by 1 | PDF Full-text (2127 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
8-Nitroguanine (8-nitroG) is a major mutagenic nucleobase lesion generated by peroxynitrite during inflammation and has been used as a potential biomarker to evaluate inflammation-related carcinogenesis. Here, we present an online solid-phase extraction (SPE) LC-MS/MS method with 6-methoxy-2-naphthyl glyoxal hydrate (MTNG) derivatization for a
[...] Read more.
8-Nitroguanine (8-nitroG) is a major mutagenic nucleobase lesion generated by peroxynitrite during inflammation and has been used as a potential biomarker to evaluate inflammation-related carcinogenesis. Here, we present an online solid-phase extraction (SPE) LC-MS/MS method with 6-methoxy-2-naphthyl glyoxal hydrate (MTNG) derivatization for a sensitive and precise measurement of 8-nitroG in DNA. Derivatization optimization revealed that an excess of MTNG is required to achieve complete derivatization in DNA hydrolysates (MTNG: 8-nitroG molar ratio of 3740:1). The use of online SPE effectively avoided ion-source contamination from derivatization reagent by washing away all unreacted MTNG before column chromatography and the ionization process in mass spectrometry. With the use of isotope-labeled internal standard, the detection limit was as low as 0.015 nM. Inter- and intraday imprecision was <5.0%. This method was compared to a previous direct LC-MS/MS method without derivatization. The comparison showed an excellent fit and consistency, suggesting that the present method has satisfactory effectiveness and reliability for 8-nitroG analysis. This method was further applied to determine the 8-nitroG in human urine. 8-NitroG was not detectable using LC-MS/MS with derivatization, whereas a significant false-positive signal was detected without derivatization. It highlights the use of MTNG derivatization in 8-nitroG analysis for increasing the method specificity. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
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Figure 1a

Open AccessArticle Graphene-Derivatized Silica Composite as Solid-Phase Extraction Sorbent Combined with GC–MS/MS for the Determination of Polycyclic Musks in Aqueous Samples
Molecules 2018, 23(2), 318; https://doi.org/10.3390/molecules23020318
Received: 6 January 2018 / Revised: 25 January 2018 / Accepted: 1 February 2018 / Published: 2 February 2018
PDF Full-text (4074 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
Polycyclic musks (PCMs) have recently received growing attention as emerging contaminants because of their bioaccumulation and potential ecotoxicological effects. Herein, an effective method for the determination of five PCMs in aqueous samples is presented. Reduced graphene oxide-derivatized silica (rGO@silica) particles were prepared from
[...] Read more.
Polycyclic musks (PCMs) have recently received growing attention as emerging contaminants because of their bioaccumulation and potential ecotoxicological effects. Herein, an effective method for the determination of five PCMs in aqueous samples is presented. Reduced graphene oxide-derivatized silica (rGO@silica) particles were prepared from graphene oxide and aminosilica microparticles and characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. PCMs were preconcentrated using rGO@silica as the solid-phase extraction sorbent and quantified by gas chromatography–tandem mass spectrometry. Several experimental parameters, such as eluent, elution volume, sorbent amount, pH, and sample volume were optimized. The correlation coefficient (R) ranged from 0.9958 to 0.9992, while the limits of detection and quantitation for the five PCMs were 0.3–0.8 ng/L and 1.1–2.1 ng/L, respectively. Satisfactory recoveries were obtained for tap water (86.6–105.9%) and river water samples (82.9–107.1%), with relative standard deviations <10% under optimal conditions. The developed method was applied to analyze PCMs in tap and river water samples from Beijing, China. Galaxolide (HHCB) and tonalide (AHTN) were the main PCM components detected in one river water sample at concentrations of 18.7 for HHCB, and 11.7 ng/L for AHTN. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
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Graphical abstract

Planned Papers

The below list represents only planned manuscripts. Some of these manuscripts have not been received by the Editorial Office yet. Papers submitted to MDPI journals are subject to peer-review.

Title: Performance Comparison between Equilibrium and Exhaustive Extraction using Sol-gel Carbowax 20M Coated Fabric Phase Sorptive Extraction Media, Classical C18 Solid Phase Extraction Sorbent and Novel Sol-gel Carbowax 20M Solid Phase Extraction Sorbent for the Extraction of Three Inflammatory Bowel Disease Treatment Drugs Residues
Authors: Marcello Locatelli1,*Abuzar Kabir2,**, Kenneth G. Furton2, Daniela Macerola1, Angela Tartaglia1, Elena Sperandio1, Silvia Piccolantonio1, Hail Ibrahim Ulusoy3,Victoria F. Samanidou4

Affiliation: 1 University of Chieti–Pescara “G. d’Annunzio”; Department of Pharmacy; Chieti; Italy;
2 International Forensic Research Institute, Department of Chemistry and Biochemistry, Florida International University, Miami, FL, USA;
3 Cumhuriyet University; Faculty of Pharmacy; Department of Analytical Chemistry; Sivas; Turkey
4 Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece;
Corresponding Authors: *Tel.: +39-0871-3554590; Fax: +39-0871-3554911; E-mail: m.locatelli@unich.it (Marcello Locatelli); ** Tel.: +1-305 348 2396; Fax: +1-305 348 4172; E-mail: akabir@fiu.edu (Abuzar Kabir)
Abstract: This paper reports the performance comparison between equilibrium and exhaustive extraction using sol-gel Carbowax 20M (sol-gel CW 20M) coated fabric phase sorptive extraction (FPSE),  classical C18 solid phase extraction (SPE) sorbent  and novel sol-gel CW 20M SPE sorbent for the simultaneous extraction and analysis of three drugs (ciprofloxacin, sulfasalazine, and cortisone) generally administered in human patients to treat inflammatory bowel disease (IBD) that possess a wide range of polarity (logP values ranging from 2.3 for Ciprofloxacin, to 1.66 for Cortisone, and 2.92 for Sulfasalazine). FPSE were carried out under equilibrium extraction mode. Both the commercial C18 SPE phases and in-house synthesized sol-gel CW 20M SPE phases were loaded in SPE cartidges and the extractions were carried out under exhaustive extraction mode. The drugs were resolved using a Luna C18 column (250 mm × 4.6 mm; 5 m particle size) in gradient elution mode within 20 minutes and the method were validated in compliance with International Guidelines for the Bioanalytical Method Validation. Novel in-house synthesized and loaded sol-gel CW 20M SPE sorbent SPE cartridges were characterized in terms of extraction capability, breakthough volume, retention volume, hold-up volume, number of theoretical plate, and retention factor. To the best of our knowledge, this is the first comprehensive comparison between equilibrium and exhaustive extraction modes as well as between classical C18 SPE sorbent, novel sol-gel CW20M SPE sorbent and sol-gel CW 20M coated FPSE media for the determination of IBD drugs, which possess a wide range of polarity and thereby poses enormous challenge for their simultaneous extraction and preconcentration at their trace and ultra-trace level concentrations.
Keywords: FPSE; in-house loaded SPE; HPLC-PDA; method validation; IBD; extraction comparison

Title: In-syringe micro solid-phase extraction for separation and preconcetration of parabens in environmental water samples
Authors: Geaneth P. Mashile, Anele Mpupa, Philiswa N. Nomngongo
Abstract: In this study, a simple, rapid and miniaturized in-syringe micro-solid phase extraction (MSPE) method was developed for separation and preconcetration of parabens (methylparaben, ethylparaben ,propylparaben and butyl paraben) in environmental water samples prior to high performance liquid chromatography photo diode array detector (HPLC-PDA). Chitosan coated activated carbon (CAC) was used as the sorbent in the in-syringe MSPE device. A response surface methodology based on central composite design was used for the optimization of factors (eluent solvent type, eluent volume, number of elution cycles, sample volume, sample pH) affecting the extraction efficiency and preconcentration procedure. The adsorbent used displayed excellent absorption performance and the adsorption capacity ranged from 156-189 mg/g. Under the optimal conditions the dynamic linear range and detection limits were 0.04-250 µg/L and 0.012-0.027 µg/L. Furthermore, for the analysis of real samples, the recoveries ranged between from 96.7 to 107 % and relative standard deviations below 5%. In conclusion CAC based in-syringe MSPE method demonstrated great potential for preconcentration of parabens in complex environmental water.

Title: Highly stable Zr(IV)-based porphyrinic metal−organic frameworks as an adsorbent for effective removal of gatifloxacin from aqueous solution

Authors: Jing-Jing Chena, Li-Juan Wanga, Gui-Ju Xua, Ru-Song Zhao a,*, Jin-Ming Linb
Affiliation: a Key Laboratory for Applied Technology of Sophisticated Analytical Instruments of Shandong Province, Analysis and Test Center, Shandong Academy of Sciences, Jinan, China
b Department of Chemistry, Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Tsinghua University, Beijing, China
* Corresponding author:Prof. R.-S. Zhao, Tel.: +86-0531-82605340; E-mail address: zhaors1976@126.com
Abstract: Water stable Zr-MOF nanoparticles (PCN-224 NPs) has been solvothermally synthesized, which shows spherical shape with smooth surface and a size of about 200 nm. PCN-224 NPs can be stable in acid and weak alkaline solution, as confirmed by powder x-ray diffraction. Gatifloxacin (GTF) adsorption measurements indicate that PCN-224 NPs exhibits high adsorption capacity of 876 mg·g-1. Meanwhile the adsorption factors, adsorption characteristics and mechanisms of GTF, were investigated in batch adsorption experiments.
Keywords: Zr(IV)-based porphyrinic metal−organic frameworks; Gatifloxacin; Removal

Title: Sensitive detection of 8-nitroguanine in DNA by chemical derivatization coupled with online solid-phase extraction LC-MS/MS
Authors: Chiung-Wen Hu a,1, Yuan-Jhe Chang b,1, Jian-Lian Chen c, Yu-Wen Hsu b,d, and Mu-Rong Chao b,e,*
Affiliation: a Department of Public Health, Chung Shan Medical University, Taichung 402, Taiwan
b Department of Occupational Safety and Health, Chung Shan Medical University, Taichung, 402, Taiwan
c School of Pharmacy, China Medical University, Taichung 404, Taiwan
d Department of Optometry, Da-Yeh University, Changhua 515, Taiwan
e Department of Occupational Medicine, Chung Shan Medical University Hospital, Taichung 402, Taiwan
* Corresponding author. Dr. Mu-Rong Chao, Department of Occupational Safety and Health, Chung Shan Medical University, No.110, Sec.1, Chien-Kuo N Road, Taichung 402, Taiwan.
Tel.: +886-4-24730022, ext. 12116; fax: +886-4-23248194. E-mail address:chaomurong@gmail.com; mrchao@csmu.edu.tw.
1 Chiung-Wen Hu and Yuan-Jhe Chang contributed equally to this work.
Abstract 8-Nitroguanine (8-nitroG) is a major mutagenic nucleobase lesion generated by peroxynitrite during inflammation and has been used as a potential biomarker to evaluate inflammation-related carcinogenesis. Here, we present an online solid-phase extraction LC-MS/MS method with 6-methoxy-2-naphthyl glyoxal hydrate (MTNG) derivatization for a sensitive and precise measurement of 8-nitroG in DNA. Derivatization optimization revealed that an excess of MTNG is required to achieve complete derivatization in DNA hydrolysates (MTNG:8-nitroG molar ratio of 3740:1). The use of online SPE effectively avoided ion-source contamination from derivatization reagent by washing away all unreacted MTNG before column chromatography and the ionization process in mass spectrometry. With the use of isotope-labeled internal standard, the detection limit was as low as 0.015 nM. Inter- and intraday imprecision was <5.0%. We measured various 8-nitroG levels in calf thymus DNA pretreated with peroxynitrite, and the results clearly showed that 8-nitroG levels increased with a peroxynitrite dose dependency. The present method was compared to a previous direct LC-MS/MS method without chemical derivatization. The comparison showed an excellent fit and consistency, suggesting that the present method has satisfactory effectiveness and reliability for 8-nitroG analysis. The present method was further applied to determine the 8-nitroG in human urine. 8-NitroG was not detectable using LC-MS/MS with derivatization, whereas a significant false-positive signal was detected without derivatization. It highlights the use of MTNG derivatization in 8-nitroG analysis for increasing the method specificity.
Keywords: LC-MS/MS, peroxynitrite, nitrated DNA lesion, derivatization, isotope-dilution

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