Analytica Chimica Acta: X最新文献

{"title":"Reconciling the pHe measurements of bioethanol: pHabs measurements of buffered 50-50 wt% water-ethanol mixtures","authors":"L. Deleebeeck ,&nbsp;A. Snedden ,&nbsp;D. Stoica","doi":"10.1016/j.acax.2022.100085","DOIUrl":"https://doi.org/10.1016/j.acax.2022.100085","url":null,"abstract":"<div><p>Water-ethanol mixtures intended for specific purposes, such as bioethanol fuel, can be subject to national quality standards, including the measurement of pHe – a solvent-specific quantification of acidity. This work discusses the shortcomings of the use of pHe in these quality standards, including the lack of metrological traceability of pHe measurements made using combination pH electrodes calibrated using aqueous pH buffers. The feasibility of measuring the acidity of 50-50 wt% water-ethanol mixtures on a non-solvent-specific, unified pH scale, which is traceable to the conventional aqueous pH scale (<span><math><mrow><msubsup><mtext>pH</mtext><mtext>abs</mtext><mrow><msub><mtext>H</mtext><mn>2</mn></msub><mtext>O</mtext></mrow></msubsup></mrow></math></span>) is demonstrated. <span><math><mrow><msubsup><mtext>pH</mtext><mtext>abs</mtext><mrow><msub><mtext>H</mtext><mn>2</mn></msub><mtext>O</mtext></mrow></msubsup></mrow></math></span> measurements of buffered and un-buffered water-ethanol mixtures using two cell configurations, including the use of an ionic liquid salt bridge (ILSB), show good agreement. The cell configuration, consisting of a commercial glass (half-cell) electrode and a reference electrode incorporating an ILSB, can be readily adopted by measurement laboratories.</p></div>","PeriodicalId":241,"journal":{"name":"Analytica Chimica Acta: X","volume":"10 ","pages":"Article 100085"},"PeriodicalIF":2.5,"publicationDate":"2022-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9240372/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"1810427","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Electrochemical application of cobalt nanoparticles-polypyrrole composite modified electrode for the determination of phoxim","authors":"Molla Tefera ,&nbsp;Merid Tessema ,&nbsp;Shimelis Admassie ,&nbsp;Meryck Ward ,&nbsp;Lisebo Phelane ,&nbsp;Emmanuel I. Iwuoha ,&nbsp;Priscilla G.L. Baker","doi":"10.1016/j.acax.2021.100077","DOIUrl":"https://doi.org/10.1016/j.acax.2021.100077","url":null,"abstract":"<div><p>In this study, cobalt nanoparticles (CoNPs) were synthesized and cobalt nanoparticles modified glassy carbon electrode (CoNPs/GCE) was prepared by drop coating the nanoparticles on glassy carbon electrode. After preparing polypyrrole modified glassy carbon electrode (PPy/GCE) using electropolymerization of pyrrole in LiClO₄ solution, cobalt nanoparticles-polypyrrole composite modified glassy carbon electrode (CoNPs/PPy/GCE) was fabricated by drop coating the CoNPs on the PPy/GCE. Different characterization techniques such as scanning electron microscopy, transmission electron microscopy, energy dispersive spectroscopy, FTIR spectroscopy, electrochemical impedance spectroscopy and cyclic voltammetry were used to study the morphological structure and electrochemical behavior of the sensors. The results demonstrated that PPy chains interacted with CoNPs through donor-acceptor bonds. Among all the electrodes, CoNPs/PPy/GCE exhibited highest electroactive surface area and lowest electron transfer resistance towards phoxim. Under the optimal conditions, the sensor showed linear relationship between the reduction peak current and the concentration of phoxim in the range of 0.025 μM–12 μM with the detection limit as 4.5 nM. Besides, the composite electrode demonstrated excellent reproducibility, good stability and selectivity towards the possible interfering substances. All of these properties made CoNPs/PPy/GCE a suitable electrochemical sensor for the electrochemical determination of phoxim in water samples using square wave voltammetry.</p></div>","PeriodicalId":241,"journal":{"name":"Analytica Chimica Acta: X","volume":"9 ","pages":"Article 100077"},"PeriodicalIF":2.5,"publicationDate":"2021-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8482437/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"2068025","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Differential light scattering and the measurement of molecules and nanoparticles: A review","authors":"Philip J. Wyatt","doi":"10.1016/j.acax.2021.100070","DOIUrl":"https://doi.org/10.1016/j.acax.2021.100070","url":null,"abstract":"<div><p>Within the past few decades, the application of light scattering techniques to a broad range of scientific disciplines has increased significantly, especially in the field of analytical chemistry. The resulting interest in and use of light scattering methods suggests the need for an easily understood introduction and review of material for those new to the method as well as for current users in need of a refresher. In many respects, the theory and its applications may appear so overwhelming for many studying the field for the first time, that they rarely can spend the time just needed to understand the basic measurements and their interpretations. A variety of applications in analytical chemistry especially have resulted in a greater understanding of many of the macromolecular processes themselves from molar mass distributions, to the macromolecular interactions responsible for aggregation processes, to determinations of structure and function. The use of such analytical processes to obtain a better understanding of nanoparticle structure and function has become almost universal.</p></div>","PeriodicalId":241,"journal":{"name":"Analytica Chimica Acta: X","volume":"7 ","pages":"Article 100070"},"PeriodicalIF":2.5,"publicationDate":"2021-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.acax.2021.100070","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"2484900","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Ex vivo Comprehensive Multiphase NMR of whole organisms: A complementary tool to in vivo NMR","authors":"Rajshree Ghosh Biswas ,&nbsp;Blythe Fortier-McGill ,&nbsp;Mohammad Akhter ,&nbsp;Ronald Soong ,&nbsp;Paris Ning ,&nbsp;Monica Bastawrous ,&nbsp;Amy Jenne ,&nbsp;Daniel Schmidig ,&nbsp;Peter De Castro ,&nbsp;Stephan Graf ,&nbsp;Till Kuehn ,&nbsp;Falko Busse ,&nbsp;Jochem Struppe ,&nbsp;Michael Fey ,&nbsp;Hermann Heumann ,&nbsp;Holger Boenisch ,&nbsp;Marcel Gundy ,&nbsp;Myrna J. Simpson ,&nbsp;André J. Simpson","doi":"10.1016/j.acax.2020.100051","DOIUrl":"https://doi.org/10.1016/j.acax.2020.100051","url":null,"abstract":"<div><p>Nuclear Magnetic Resonance (NMR) spectroscopy is a non-invasive analytical technique which allows for the study of intact samples. Comprehensive Multiphase NMR (CMP-NMR) combines techniques and hardware from solution state and solid state NMR to allow for the holistic analysis of all phases (i.e. solutions, gels and solids) in unaltered samples. This study is the first to apply CMP-NMR to deceased, intact organisms and uses ¹³C enriched <em>Daphnia magna</em> (water fleas) as an example. <em>D. magna</em> are commonly used model organisms for environmental toxicology studies. As primary consumers, they are responsible for the transfer of nutrients across trophic levels, and a decline in their population can potentially impact the entire freshwater aquatic ecosystem. Though <em>in vivo</em> research is the ultimate tool to understand an organism’s most biologically relevant state, studies are limited by conditions (i.e. oxygen requirements, limited experiment time and reduced spinning speed) required to keep the organisms alive, which can negatively impact the quality of the data collected. In comparison, <em>ex vivo</em> CMP-NMR is beneficial in that; organisms do not need oxygen (eliminating air holes in rotor caps and subsequent evaporation); samples can be spun faster, leading to improved spectral resolution; more biomass per sample can be analyzed; and experiments can be run for longer. In turn, higher quality <em>ex vivo</em> NMR, can provide more comprehensive NMR assignments, which in many cases could be transferred to better understand less resolved <em>in vivo</em> signals. This manuscript is divided into three sections: 1) multiphase spectral editing techniques, 2) detailed metabolic assignments of 2D NMR of ¹³C enriched <em>D. magna</em> and 3) multiphase biological changes over different life stages, ages and generations of <em>D. magna</em>. In summary, <em>ex vivo</em> CMP-NMR proves to be a very powerful approach to study whole organisms in a comprehensive manner and should provide very complementary information to <em>in vivo</em> based research.</p></div>","PeriodicalId":241,"journal":{"name":"Analytica Chimica Acta: X","volume":"6 ","pages":"Article 100051"},"PeriodicalIF":2.5,"publicationDate":"2020-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.acax.2020.100051","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"1506749","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"ANOVA simultaneous component analysis: A tutorial review","authors":"Carlo Bertinetto ,&nbsp;Jasper Engel ,&nbsp;Jeroen Jansen","doi":"10.1016/j.acax.2020.100061","DOIUrl":"https://doi.org/10.1016/j.acax.2020.100061","url":null,"abstract":"<div><p>When analyzing experimental chemical data, it is often necessary to incorporate the structure of the study design into the chemometric/statistical models to effectively address the research questions of interest. ANOVA-Simultaneous Component Analysis (ASCA) is one of the most prominent methods to include such information in the quantitative analysis of multivariate data, especially when the number of variables is large. This tutorial review intends to explain in a simple way how ASCA works, how it is operated and how to correctly interpret ASCA results, with approachable mathematical and visual descriptions. Two examples are given: the first, a simulated chemical reaction, serves to illustrate the ASCA steps and the second, from a real chemical ecology data set, the interpretation of results. An overview of methods closely related to ASCA is also provided, pointing out their differences and scope, to give a wide-ranging picture of the available options to build multivariate models that take experimental design into account.</p></div>","PeriodicalId":241,"journal":{"name":"Analytica Chimica Acta: X","volume":"6 ","pages":"Article 100061"},"PeriodicalIF":2.5,"publicationDate":"2020-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.acax.2020.100061","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"1506753","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Analysis of total microcystins and nodularins by oxidative cleavage of their ADMAdda, DMAdda, and Adda moieties","authors":"Amanda J. Foss ,&nbsp;Christopher O. Miles ,&nbsp;Alistair L. Wilkins ,&nbsp;Frode Rise ,&nbsp;Kristian W. Trovik ,&nbsp;Kamil Cieslik ,&nbsp;Mark T. Aubel","doi":"10.1016/j.acax.2020.100060","DOIUrl":"https://doi.org/10.1016/j.acax.2020.100060","url":null,"abstract":"<div><p>Microcystins (MCs) and nodularins (NODs) exhibit high structural variability, including modifications of the Adda (3<em>S</em>-amino-9<em>S</em>-methoxy-2<em>S</em>,6,8<em>S</em>-trimethyl-10-phenyldeca-4<em>E</em>,6<em>E</em>-dienoic acid) moiety. Variations include 9-<em>O</em>-desmethylAdda (DMAdda) and 9-<em>O</em>-acetylDMAdda (ADMAdda) which, unless targeted, may go undetected. Therefore, reference standards were prepared of [ADMAdda⁵]MCs and [DMAdda⁵]MCs, which were analyzed using multiple approaches. The cross-reactivities of the [DMAdda⁵]- and [ADMAdda⁵]MC standards were similar to that of MC-LR when analyzed with a protein phosphatase 2A (PP2A) inhibition assay, but were &lt;0.25% when analyzed with an Adda enzyme-linked immunosorbent assay (ELISA). Oxidative cleavage experiments identified compounds that could be used in the analysis of total MCs/NODs in a similar fashion to the 2<em>R</em>-methyl-3<em>S</em>-methoxy-4-phenylbutanoic acid (MMPB) technique. Products from oxidative cleavage of both the 4,5- and 6,7-ene of Adda, DMAdda and ADMAdda were observed, and three oxidation products, one from each Adda variant, were chosen for analysis and applied to three field samples and a <em>Nostoc</em> culture. Results from the oxidative cleavage method for total Adda, DMAdda, and ADMAdda were similar to those from the Adda-ELISA, PP2A inhibition, and LC-MS/MS analyses, except for the <em>Nostoc</em> culture where the Adda-ELISA greatly underestimated microcystin levels. This oxidative cleavage method can be used for routine analysis of field samples and to assess the presence of the rarely reported, but toxic, DMAdda/ADMAdda-containing MCs and NODs.</p></div>","PeriodicalId":241,"journal":{"name":"Analytica Chimica Acta: X","volume":"6 ","pages":"Article 100060"},"PeriodicalIF":2.5,"publicationDate":"2020-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.acax.2020.100060","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"1746875","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Experimental determination of the bioluminescence resonance energy transfer (BRET) Förster distances of NanoBRET and red-shifted BRET pairs","authors":"Felix Weihs ,&nbsp;Jian Wang ,&nbsp;Kevin D.G. Pfleger ,&nbsp;Helen Dacres","doi":"10.1016/j.acax.2020.100059","DOIUrl":"https://doi.org/10.1016/j.acax.2020.100059","url":null,"abstract":"<div><p>Bioluminescence Resonance Energy Transfer (BRET) is widely applied to study protein-protein interactions, as well as increasingly to monitor both ligand binding and molecular rearrangements. The Förster distance (R₀) describes the physical distance between the two chromophores at which 50% of the maximal energy transfer occurs and it depends on the choice of RET components. R₀ can be experimentally determined using flexible peptide linkers of known lengths to separate the two chromophores. Knowledge of the R₀ helps to inform on the choice of BRET system. For example, we have previously shown that BRET² exhibits the largest R₀ to date for any genetically encoded RET pair, which may be advantageous for investigating large macromolecular complexes if its issues of low and fast-decaying bioluminescence signal can be accommodated.</p><p>In this study we have determined R₀ for a range of bright and red-shifted BRET pairs, including NanoBRET with tetramethylrhodamine (TMR), non-chloro TOM (NCT), mCherry or Venus as acceptor, and BRET⁶, a red-shifted BRET²-like system. This study revealed R₀ values of 6.15 nm and 6.94 nm for NanoBRET using TMR or NCT as acceptor ligands, respectively. R₀ was 5.43 nm for NanoLuc-mCherry, 5.59 nm for NanoLuc-Venus and 5.47 nm for BRET⁶. This extends the palette of available BRET Förster distances, to give researchers a better-informed choice when considering BRET systems and points towards NanoBRET with NCT as a good alternative to BRET² as an analysis tool for large macromolecular complexes.</p></div>","PeriodicalId":241,"journal":{"name":"Analytica Chimica Acta: X","volume":"6 ","pages":"Article 100059"},"PeriodicalIF":2.5,"publicationDate":"2020-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.acax.2020.100059","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"1969173","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Evaluation of CRM homogeneity in cases of insufficient method repeatability: Comparison of Bayesian analysis with substitutes for ANOVA based estimates","authors":"Thomas P.J. Linsinger","doi":"10.1016/j.acax.2020.100049","DOIUrl":"https://doi.org/10.1016/j.acax.2020.100049","url":null,"abstract":"<div><p>Insufficient method repeatability is a problem characterising the evaluation of certified reference materials (CRMs). In investigating the homogeneity studies of 216 certified parameters from 36 CRMs released by the European Commission’s Joint Research Centre (JRC) over the last four years, it was found that in 1/3 of the cases, the method repeatability (<em>s</em>_r) was too high to calculate the standard deviation between units (<em>s</em>_bb) by classical analysis of variance (ANOVA). It was also found that the application of the repeatability requirement stated in the ISO Guide 35:2017 is not feasible since it would require unrealistically low repeatability standard deviations or an impossibly high number of replicates per unit.</p><p>Evaluation of the uncertainty of homogeneity (<em>u</em>_bb) as evaluated by ANOVA using both the maximum of <em>s</em>_bb and 0, the maximum of <em>s</em>_bb and <em>u</em>∗_bb, the uncertainty hidden by method repeatability, the maximum of <em>s</em>_bb and <em>s</em>_bb/√n and Bayesian analysis, using both informative and diffuse priors, as well as the standard deviation of the unit means, were compared using simulated homogeneity studies with repeatabilities of 1–8% and <em>s</em>_bb between 0.2 and 2.8%. It was found that using the maximum of <em>s</em>_bb and <em>s</em>_bb/√n as an estimate of <em>u</em>_bb guards against severe underestimation but usually results in a severe overestimation of the between-unit variation. Using the maximum of (<em>s</em>_bb, 0) shows the least average bias but results in a severe underestimation of <em>u</em>_bb in a high fraction of cases. Using the maximum of (<em>s</em>_bb, <em>u</em>∗_bb) limits, but does not completely eliminate cases of a severe underestimation. Also, it leads to average results biased towards high values. For the range of <em>s</em>_bb and <em>s</em>_r investigated, Bayesian analysis performed worse than max (<em>s</em>_bb, <em>u</em>∗_bb) in limiting severe underestimation of <em>u</em>_bb, but limited the average bias towards high results.</p><p>A risk-based approach to cases of insufficient method repeatability is proposed where, after evaluating the other contributions to the uncertainty of certified values, the effect of severe over- and underestimation of <em>u</em>_bb is evaluated, and an appropriate approach is chosen based on this analysis.</p></div>","PeriodicalId":241,"journal":{"name":"Analytica Chimica Acta: X","volume":"5 ","pages":"Article 100049"},"PeriodicalIF":2.5,"publicationDate":"2020-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.acax.2020.100049","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"2098893","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Oligonucleotide hybridization with magnetic separation assay for multiple SNP phasing","authors":"Henson L. Lee Yu,&nbsp;Tsz Wing Fan,&nbsp;I-Ming Hsing","doi":"10.1016/j.acax.2020.100050","DOIUrl":"https://doi.org/10.1016/j.acax.2020.100050","url":null,"abstract":"<div><p>Since humans have two copies of each gene, multiple mutations in different loci may or may not be found on the same strand of DNA (i.e., inherited from one parent). When a person is heterozygous at more than one position, the placement of these mutations, also called the haplotype phase, (i.e., <em>cis</em> for the same strand and <em>trans</em> for different strands) can result in the expression of different amount and type of proteins. In this work, we described an enzyme-free method to phase two single nucleotide polymorphisms (SNPs) using two fluorophore/quencher-labelled probes, where one of which was biotinylated. The fluorescence signal was obtained twice: first, after the addition of the labelled probes and second, after the addition of the magnetic beads. The first signal was shown to be proportional to the total number of SNP A and SNP B present in the target analyte, while the second signal showed a marked decrease of the fluorescence signal from the non-biotinylated probe when the SNPs were in <em>trans</em>, showing that the probe immobilized on the magnetic bead selectively captures targets with SNPs in a <em>cis</em> configuration. We then mimic the nature of the human genome which consists of two haplotype copies of each gene, and showed that 250 nM of the 10 possible pairs of haplotypes could be differentiated using a combination of fluorescence microscopy and fluorescence detection.</p></div>","PeriodicalId":241,"journal":{"name":"Analytica Chimica Acta: X","volume":"5 ","pages":"Article 100050"},"PeriodicalIF":2.5,"publicationDate":"2020-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.acax.2020.100050","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"1895109","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Selective pressurized liquid extraction of plant secondary metabolites: Convallaria majalis L. as a case","authors":"Xiaomeng Liang,&nbsp;Nikoline Juul Nielsen,&nbsp;Jan H. Christensen","doi":"10.1016/j.acax.2020.100040","DOIUrl":"https://doi.org/10.1016/j.acax.2020.100040","url":null,"abstract":"<div><p>A fast and efficient selective pressurized liquid extraction (sPLE) method was developed to extract secondary metabolites from complex plant matrix. <em>Convallaria majalis</em> L., a plant producing toxic steroids, was used as proof-of-concept. The method was optimized in the aspects of preheating, dispersant, extraction temperature and solvent, and the use of C18 as in-cell cleanup sorbent. Eight authentic natural steroids with diverse sugar moieties and hydrophobicities were selected as reference analytes and spiked to 0.1 g dried leaves. The extraction performance was evaluated based on the analytes’ stability, recovery, matrix effect in the electrospray interface and the level of co-extractives. With the optimal method, the extraction was finished in 10 min. A colorless extract was obtained with recoveries ranging from 63% to 107% and absolute matrix effects ranging from 3% to 27%. The optimized method was validated by extracting 0.1 g, 0.2 g and 0.4 g spiked plant samples; method accuracy and precision were assessed by recoveries and relative standard deviations of the combined extraction-analysis workflow. The method was also tested on soil samples and indicated its suitability for measuring secondary metabolites in multiple environmental matrices. To our knowledge, this is the first time sPLE has been reported to extract plant secondary metabolites from a complex plant matrix, with satisfactory recoveries and low matrix effects. This is also the first time (s)PLE has been reported to extract plant secondary metabolites from soil. We envision the method be coupled with liquid chromatography-electrospray ionization-high resolution mass spectrometry in a standard metabolomics workflow to facilitate plant metabolomics studies.</p></div>","PeriodicalId":241,"journal":{"name":"Analytica Chimica Acta: X","volume":"4 ","pages":"Article 100040"},"PeriodicalIF":2.5,"publicationDate":"2020-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.acax.2020.100040","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"1746878","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}