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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: closed (28 February 2019) | Viewed by 60270

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Guest Editor
Laboratory of Analytical Chemistry, School of Chemistry, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece
Interests: analytical chemistry; sample preparation; chromatography; HPLC; method validation; method development; separation science; food analysis; bioanalysis; environmental analysis; green analytical chemistry; sorptive extraction; microextraction techniques
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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

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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 (13 papers)

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Research

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9 pages, 1303 KiB  
Article
Synthetic Peptide Purification via Solid-Phase Extraction with Gradient Elution: A Simple, Economical, Fast, and Efficient Methodology
by Diego Sebastián Insuasty Cepeda, Héctor Manuel Pineda Castañeda, Andrea Verónica Rodríguez Mayor, Javier Eduardo García Castañeda, Mauricio Maldonado Villamil, Ricardo Fierro Medina and Zuly Jenny Rivera Monroy
Molecules 2019, 24(7), 1215; https://doi.org/10.3390/molecules24071215 - 28 Mar 2019
Cited by 27 | Viewed by 6815
Abstract
A methodology was implemented for purifying peptides in one chromatographic run via solid-phase extraction (SPE), reverse phase mode (RP), and gradient elution, obtaining high-purity products with good yields. Crude peptides were analyzed by reverse phase high performance liquid chromatography and a new mathematical [...] Read more.
A methodology was implemented for purifying peptides in one chromatographic run via solid-phase extraction (SPE), reverse phase mode (RP), and gradient elution, obtaining high-purity products with good yields. Crude peptides were analyzed by reverse phase high performance liquid chromatography and a new mathematical model based on its retention time was developed in order to predict the percentage of organic modifier in which the peptide will elute in RP-SPE. This information was used for designing the elution program of each molecule. It was possible to purify peptides with different physicochemical properties, showing that this method is versatile and requires low solvent consumption, making it the least polluting one. Reverse phase-SPE can easily be routinely implemented. It is an alternative to enrich and purified synthetic or natural molecules. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
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16 pages, 2873 KiB  
Article
Rapid Monitoring of Organochlorine Pesticide Residues in Various Fruit Juices and Water Samples Using Fabric Phase Sorptive Extraction and Gas Chromatography-Mass Spectrometry
by Ramandeep Kaur, Ripneel Kaur, Susheela Rani, Ashok Kumar Malik, Abuzar Kabir, Kenneth G. Furton and Victoria F. Samanidou
Molecules 2019, 24(6), 1013; https://doi.org/10.3390/molecules24061013 - 13 Mar 2019
Cited by 25 | Viewed by 4603
Abstract
Fabric phase sorptive extraction, an innovative integration of solid phase extraction and solid phase microextraction principles, has been combined with gas chromatography-mass spectrometry for the rapid extraction and determination of nineteen organochlorine pesticides in various fruit juices and water samples. FPSE consolidates the [...] Read more.
Fabric phase sorptive extraction, an innovative integration of solid phase extraction and solid phase microextraction principles, has been combined with gas chromatography-mass spectrometry for the rapid extraction and determination of nineteen organochlorine pesticides in various fruit juices and water samples. FPSE consolidates the advanced features of sol-gel derived extraction sorbents with the rich surface chemistry of cellulose fabric substrate, which could extract the target analytes directly from the complex sample matrices, substantially simplifying the sample preparation operation. Important FPSE parameters, including sorbent chemistry, extraction time, stirring speed, type and volume of back-extraction solvent, and back-extraction time have been optimized. Calibration curves were obtained in a concentration range of 0.1–500 ng/mL. Under optimum conditions, limits of detection were obtained in a range of 0.007–0.032 ng/mL with satisfactory precision (RSD < 6%). The relative recoveries obtained by spiking organochlorine pesticides in water and selected juice samples were in the range of 91.56–99.83%. The sorbent sol-gel poly(ethylene glycol)-poly(propylene glycol)-poly(ethylene glycol) was applied for the extraction and preconcentration of organochlorine pesticides in aqueous and fruit juice samples prior to analysis with gas chromatography-mass spectrometry. The results demonstrated that the present method is simple, rapid, and precise for the determination of organochlorine pesticides in aqueous samples. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
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14 pages, 1716 KiB  
Article
Comparison between Exhaustive and Equilibrium Extraction Using Different SPE Sorbents and Sol-Gel Carbowax 20M Coated FPSE Media
by Angela Tartaglia, Marcello Locatelli, Abuzar Kabir, Kenneth G. Furton, Daniela Macerola, Elena Sperandio, Silvia Piccolantonio, Halil I. Ulusoy, Fabio Maroni, Pantaleone Bruni, Fausto Croce and Victoria F. Samanidou
Molecules 2019, 24(3), 382; https://doi.org/10.3390/molecules24030382 - 22 Jan 2019
Cited by 16 | Viewed by 3643
Abstract
This paper reports the performance comparison between the exhaustive and equilibrium extraction using classical Avantor C18 solid phase extraction (SPE) sorbent, hydrophilic-lipophilic balance (HLB) SPE sorbent, Sep-Pak C18 SPE sorbent, novel sol-gel Carbowax 20M (sol-gel CW 20M) SPE sorbent, and sol-gel CW 20M [...] Read more.
This paper reports the performance comparison between the exhaustive and equilibrium extraction using classical Avantor C18 solid phase extraction (SPE) sorbent, hydrophilic-lipophilic balance (HLB) SPE sorbent, Sep-Pak C18 SPE sorbent, novel sol-gel Carbowax 20M (sol-gel CW 20M) SPE sorbent, and sol-gel CW 20M coated fabric phase sorptive extraction (FPSE) media for the simultaneous extraction and analysis of three inflammatory bowel disease (IBD) drugs that possess logP values (polarity) ranging from 1.66 for cortisone, 2.30 for ciprofloxacin, and 2.92 for sulfasalazine. Both the commercial SPE phases and in-house synthesized sol-gel CW 20M SPE phases were loaded in SPE cartridges and the extractions were carried out under an exhaustive extraction mode. FPSE was carried out under an equilibrium extraction mode. The drug compounds were resolved using a Luna C18 column (250 mm × 4.6 mm; 5 μm particle size) in gradient elution mode within 20 min and the method was validated in compliance with international guidelines for the bioanalytical method validation. Novel in-house synthesized and loaded sol-gel CW 20M SPE sorbent cartridges were characterized in terms of their extraction capability, breakthrough volume, retention volume, hold-up volume, number of the theoretical plate, and the retention factor. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
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14 pages, 1955 KiB  
Article
Influence of Ligand Functionalization of UiO-66-Based Metal-Organic Frameworks When Used as Sorbents in Dispersive Solid-Phase Analytical Microextraction for Different Aqueous Organic Pollutants
by Iván Taima-Mancera, Priscilla Rocío-Bautista, Jorge Pasán, Juan H. Ayala, Catalina Ruiz-Pérez, Ana M. Afonso, Ana B. Lago and Verónica Pino
Molecules 2018, 23(11), 2869; https://doi.org/10.3390/molecules23112869 - 3 Nov 2018
Cited by 38 | Viewed by 6153
Abstract
Four metal-organic frameworks (MOFs), specifically UiO-66, UiO-66-NH2, UiO-66-NO2, and MIL-53(Al), were synthesized, characterized, and used as sorbents in a dispersive micro-solid phase extraction (D-µSPE) method for the determination of nine pollutants of different nature, including drugs, phenols, polycyclic aromatic [...] Read more.
Four metal-organic frameworks (MOFs), specifically UiO-66, UiO-66-NH2, UiO-66-NO2, and MIL-53(Al), were synthesized, characterized, and used as sorbents in a dispersive micro-solid phase extraction (D-µSPE) method for the determination of nine pollutants of different nature, including drugs, phenols, polycyclic aromatic hydrocarbons, and personal care products in environmental waters. The D-µSPE method, using these MOFs as sorbents and in combination with high-performance liquid chromatography (HPLC) and diode-array detection (DAD), was optimized. The optimization study pointed out to UiO-66-NO2 as the best MOF to use in the multi-component determination. Furthermore, the utilization of isoreticular MOFs based on UiO-66 with the same topology but different functional groups, and MIL-53(Al) to compare with, allowed us for the first time to evaluate the influence of such functionalization of the ligand with regards to the efficiency of the D-µSPE-HPLC-DAD method. Optimum conditions included: 20 mg of UiO-66-NO2 MOF in 20 mL of the aqueous sample, 3 min of agitation by vortex and 5 min of centrifugation, followed by the use of only 500 µL of acetonitrile as desorption solvent (once the MOF containing analytes was separated), 5 min of vortex and 5 min of centrifugation. The validation of the D-µSPE-HPLC-DAD method showed limits of detection down to 1.5 ng·L−1, average relative recoveries of 107% for a spiked level of 1.50 µg·L−1, and inter-day precision values with relative standard deviations lower than 14%, for the group of pollutants considered. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
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10 pages, 5291 KiB  
Article
Determination of Enantiomeric Excess by Solid-Phase Extraction Using a Chiral Metal-Organic Framework as Sorbent
by Jun-Hui Zhang, Bo Tang, Sheng-Ming Xie, Bang-Jin Wang, Mei Zhang, Xing-Lian Chen, Min Zi and Li-Ming Yuan
Molecules 2018, 23(11), 2802; https://doi.org/10.3390/molecules23112802 - 29 Oct 2018
Cited by 8 | Viewed by 3863
Abstract
Metal-organic frameworks (MOFs) have recently attracted considerable attention because of their fascinating structures and intriguing potential applications in diverse areas. In this study, we developed a novel method for determination of enantiomeric excess (ee) of (±)-1,1′-bi-2-naphthol by solid-phase extraction (SPE) using [...] Read more.
Metal-organic frameworks (MOFs) have recently attracted considerable attention because of their fascinating structures and intriguing potential applications in diverse areas. In this study, we developed a novel method for determination of enantiomeric excess (ee) of (±)-1,1′-bi-2-naphthol by solid-phase extraction (SPE) using a chiral MOF, [Co(l-tyr)]n(l-tyrCo), as sorbent. After optimization of the experimental conditions, a good linear relationship between the ee and the absorbance of the eluate (R2 = 0.9984) was obtained and the standard curve was established at the concentration of 3 mmol L1. The ee values of (±)-1,1′-bi-2-naphthol samples can be rapidly calculated using the standard curve after determination of the absorbance of the eluate. The method showed good accuracy, with an average error of 2.26%, and is promising for ee analysis. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
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13 pages, 3802 KiB  
Article
Melamine Sponge Functionalized with Urea-Formaldehyde Co-Oligomers as a Sorbent for the Solid-Phase Extraction of Hydrophobic Analytes
by María Teresa García-Valverde, Theodoros Chatzimitakos, Rafael Lucena, Soledad Cárdenas and Constantine D. Stalikas
Molecules 2018, 23(10), 2595; https://doi.org/10.3390/molecules23102595 - 10 Oct 2018
Cited by 14 | Viewed by 3582
Abstract
A new procedure for the functionalization of melamine sponge (MeS) with urea-formaldehyde (UF) co-oligomers is put forward. The procedure differs from the typical synthesis of the UF co-polymer, as it employs a base-catalyzed condensation step at certain concentrations of urea and formaldehyde. The [...] Read more.
A new procedure for the functionalization of melamine sponge (MeS) with urea-formaldehyde (UF) co-oligomers is put forward. The procedure differs from the typical synthesis of the UF co-polymer, as it employs a base-catalyzed condensation step at certain concentrations of urea and formaldehyde. The produced melamine-urea-formaldehyde (MUF) sponge cubes are hydrophobic, despite the presence of hydrophilic groups in the oligomers. The MUF sponge developed herein is used as a sorbent for the solid-phase extraction of 10 analytes, from 6 different classes (i.e., non-steroidal anti-inflammatory drugs, benzophenones, parabens, phenols, pesticides and musks) and an analytical method is developed for their liquid chromatographic separation and detection. Low limits of quantification (0.03 and 1.0 μg L−1), wide linear ranges and excellent recoveries (92–100%) are some of the benefits of the proposed procedure. The study of the synthesis conditions of MUF cubes reveals that by altering them the hydrophilic/lipophilic balance of the MUF cubes can be tuned, hinting towards a strong potential for many other applications. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
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15 pages, 1677 KiB  
Article
In-Syringe Micro Solid-Phase Extraction Method for the Separation and Preconcentration of Parabens in Environmental Water Samples
by Geaneth Pertunia Mashile, Anele Mpupa and Philiswa Nosizo Nomngongo
Molecules 2018, 23(6), 1450; https://doi.org/10.3390/molecules23061450 - 14 Jun 2018
Cited by 24 | Viewed by 4801
Abstract
In this study, a simple, rapid and effective in-syringe micro-solid phase extraction (MSPE) method was developed for the separation and preconcetration of parabens (methyl, ethyl, propyl and butyl paraben) in environmental water samples. The parabens were determined and quantified using high performance liquid [...] Read more.
In this study, a simple, rapid and effective in-syringe micro-solid phase extraction (MSPE) method was developed for the separation and preconcetration of parabens (methyl, ethyl, propyl and butyl paraben) in environmental water samples. The parabens were determined and quantified using high performance liquid chromatography and a 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 of the preconcentration procedure. The adsorbent used displayed excellent absorption performance and the adsorption capacity ranged from 227–256 mg g−1. Under the optimal conditions the dynamic linear ranges for the parabens were between 0.04 and 380 µg L−1. The limits of detection and quantification ranged from 6–15 ng L−1 and 20–50 ng L−1, respectively. The intraday (repeatability) and interday (reproducibility) precisions expressed as relative standard deviations (%RSD) were below 5%. Furthermore, the in-syringe MSPE/HPLC procedure was validated using spiked wastewater and tap water samples and the recoveries ranged between from 96.7 to 107%. In conclusion, CAC based in-syringe MSPE method demonstrated great potential for preconcentration of parabens in complex environmental water. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
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11 pages, 1891 KiB  
Article
Carbon Nanohorn Suprastructures on a Paper Support as a Sorptive Phase
by Julia Ríos-Gómez, Beatriz Fresco-Cala, María Teresa García-Valverde, Rafael Lucena and Soledad Cárdenas
Molecules 2018, 23(6), 1252; https://doi.org/10.3390/molecules23061252 - 24 May 2018
Cited by 35 | Viewed by 3827
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)
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11 pages, 11414 KiB  
Article
Preconcentration and Determination of Perfluoroalkyl Substances (PFASs) in Water Samples by Bamboo Charcoal-Based Solid-Phase Extraction Prior to Liquid Chromatography–Tandem Mass Spectrometry
by Ze-Hui Deng, Chuan-Ge Cheng, Xiao-Li Wang, Shui-He Shi, Ming-Lin Wang and Ru-Song Zhao
Molecules 2018, 23(4), 902; https://doi.org/10.3390/molecules23040902 - 14 Apr 2018
Cited by 25 | Viewed by 5271
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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12 pages, 3123 KiB  
Article
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
by Jun Dang, Yulei Cui, Jinjin Pei, Huilan Yue, Zenggen Liu, Weidong Wang, Lijin Jiao, Lijuan Mei, Qilan Wang, Yanduo Tao and Yun Shao
Molecules 2018, 23(3), 623; https://doi.org/10.3390/molecules23030623 - 9 Mar 2018
Cited by 13 | Viewed by 3742
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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14 pages, 2127 KiB  
Article
Sensitive Detection of 8-Nitroguanine in DNA by Chemical Derivatization Coupled with Online Solid-Phase Extraction LC-MS/MS
by Chiung-Wen Hu, Yuan-Jhe Chang, Jian-Lian Chen, Yu-Wen Hsu and Mu-Rong Chao
Molecules 2018, 23(3), 605; https://doi.org/10.3390/molecules23030605 - 8 Mar 2018
Cited by 9 | Viewed by 3931
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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11 pages, 4074 KiB  
Article
Graphene-Derivatized Silica Composite as Solid-Phase Extraction Sorbent Combined with GC–MS/MS for the Determination of Polycyclic Musks in Aqueous Samples
by Cheng Li, Jiayi Chen, Yan Chen, Jihua Wang, Hua Ping and Anxiang Lu
Molecules 2018, 23(2), 318; https://doi.org/10.3390/molecules23020318 - 2 Feb 2018
Cited by 14 | Viewed by 4450
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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Review

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14 pages, 242 KiB  
Review
Solid-Phase Extraction of Polar Benzotriazoles as Environmental Pollutants: A Review
by Ida Kraševec and Helena Prosen
Molecules 2018, 23(10), 2501; https://doi.org/10.3390/molecules23102501 - 29 Sep 2018
Cited by 15 | Viewed by 3676
Abstract
Polar benzotriazoles are corrosion inhibitors with widespread use; they are environmentally characterized as emerging pollutants in the water system, where they are present in low concentrations. Various extraction methods have been used for their separation from various matrices, ranging from classical liquid–liquid extractions [...] Read more.
Polar benzotriazoles are corrosion inhibitors with widespread use; they are environmentally characterized as emerging pollutants in the water system, where they are present in low concentrations. Various extraction methods have been used for their separation from various matrices, ranging from classical liquid–liquid extractions to various microextraction techniques, but the most frequently applied extraction technique remains the solid-phase extraction (SPE), which is the focus of this review. We present an overview of the methods, developed in the last decade, applied for the determination of benzotriazoles in aqueous and solid environmental samples. Several other matrices, such as human urine and plant material, are also considered in the text. The methods are reviewed according to the determined compounds, sample matrices, cartridges and eluents used, extraction recoveries and the achieved limits of quantification. A critical evaluation of the advantages and drawbacks of the published methods is given. Full article
(This article belongs to the Special Issue Solid Phase Extraction: State of the Art and Future Perspectives)
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