Kjell Kochale , Björn Lang , Ricardo Cunha , Thorsten Teutenberg , Torsten C. Schmidt
{"title":"Online coupling of miniaturized HPLC and high performance thin layer chromatography by a fractionation unit for effect directed analysis","authors":"Kjell Kochale , Björn Lang , Ricardo Cunha , Thorsten Teutenberg , Torsten C. Schmidt","doi":"10.1016/j.sampre.2024.100102","DOIUrl":"https://doi.org/10.1016/j.sampre.2024.100102","url":null,"abstract":"<div><p>The rising discharge of anthropogenic chemicals into aquatic environments poses a significant threat, necessitating effective monitoring strategies. This study introduces an innovative approach to effect-directed analysis (EDA) by coupling liquid chromatography (LC) with high-performance thin-layer chromatography (HPTLC), utilizing a modified MALDI spotter. The objective is to optimize fractionation parameters for sample application and assess the method's viability in identifying acetylcholinesterase (AChE) inhibitors, specifically malathion, parathion, and chlorfenvinphos.</p><p>The optimization process involves controlling sample volume, spot shape, and spot distances on HPTLC plates. Successful application is demonstrated by a miniaturized LC system coupled to the HPTLC plate via spotter, allowing effective separation and identification of AChE inhibitors. The study further explores the method's application to water samples from a river with predominantly agricultural drainage area.</p><p>Spiked samples reveal distinct active spots, identified through extraction and subsequent high-resolution mass spectrometry (HRMS) measurements. However, results indicate the absence of AChE inhibitors in non-spiked water samples, affirming the efficacy of the EU ban on most organophosphate pesticides. The usefulness of HPTLC in separation of coeluting substances from HPLC is emphasized, demonstrating its suitability for the effect-directed analysis of complex samples.</p><p>This work shows the integration of HPTLC with liquid chromatography for EDA, offering a powerful tool for identifying and monitoring AChE inhibitors in water samples. The approach addresses limitations in current monitoring strategies and provides insights into the presence and impact of chemicals in aquatic ecosystems. The study contributes to ongoing efforts to enhance water quality monitoring, aligning with the principles of the EU Water Framework Directive.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"9 ","pages":"Article 100102"},"PeriodicalIF":0.0,"publicationDate":"2024-01-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000019/pdfft?md5=c7bcfd68d43ec6630ffbda237600dae0&pid=1-s2.0-S2772582024000019-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139504248","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}
Lucie K. Tintrop , Leonardo Solazzo , Amir Salemi , Maik A. Jochmann , Torsten C. Schmidt
{"title":"Characterization of a hydrophilic-lipophilic balanced SPME material for enrichment of analytes with different polarities from aqueous samples","authors":"Lucie K. Tintrop , Leonardo Solazzo , Amir Salemi , Maik A. Jochmann , Torsten C. Schmidt","doi":"10.1016/j.sampre.2023.100099","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100099","url":null,"abstract":"<div><p>The choice of the extraction material is a critical step in solid-phase microextraction (SPME), especially the extraction of analytes which strongly differ in their polarity is challenging. This study is intended to give first insights into the headspace extraction of analytes with large differences in polarity by using a novel hydrophilic-lipophilic-balanced (HLB) SPME material with different particle sizes (5 µm, 5 + 30 µm, and 30 µm) in classical SPME, as well as SPME arrow format. The obtained results were compared to conventional and already established divinylbenzene carbon wide-range polydimethylsiloxane (DVB-CWR-PDMS) and PDMS SPME arrow fibers. The chosen model analytes toluene, indole, phenol, anisole, <em>o</em>-xylene, naphthalene, 2-heptanone, n-dodecane, and lindane are assigned to different substance classes with K<sub>aw</sub> values ranging from -5.0–2.5 and K<sub>ow</sub> values from 1.5 to 7.5. The highest amount of the analytes was extracted by the HLB 5 + 30 µm arrow and the HLB 5 µm arrow, whereas the HLB SPME with a six times smaller phase volume compared to an SPME arrow, performed almost as well as the DVB-CWR-PDMS arrow. The 8-point calibration with the 5 + 30 µm HLB SPME arrow in the range of 5–70 µg L<sup>−1</sup> of the analytes showed good linearity with R<sup>2</sup> values ranging from 0.9765 to 0.9982, MDLs from 0.9 to 6.2 µg L<sup>−1</sup> and RSDs from 2 to 31 %. For all of the observed analytes, the HLB material performed better than the conventional extraction materials and has great potential to replace the conventional extraction materials in many applications.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"8 ","pages":"Article 100099"},"PeriodicalIF":0.0,"publicationDate":"2023-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582023000499/pdfft?md5=d2b8cc7bb5c8a49ef25bbcfcd22a2f90&pid=1-s2.0-S2772582023000499-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"134656632","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":"Determination of chlorophylls a and b and β-carotene in environmental waters: Diminishing wastes and analysis time by in-tube solid-phase microextraction coupled on-line to nano liquid chromatography","authors":"C. Soto, R. Herráez-Hernández, P. Campíns-Falcó","doi":"10.1016/j.sampre.2023.100093","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100093","url":null,"abstract":"<div><p>Chlorophylls and carotenoids are indicators of water quality. A new method based on in-tube solid-phase microextraction (IT-SPME) coupled on-line to nano-liquid chromatography with diode array detection (NanoLC-DAD) was developed. This paper aims to provide selectivity and sensitivity with a short analysis time of about 10 min and low residues of friendly solvents, 5 µL/run of ethanol:water 95:5 and 250 µL of ethanol for dissolving the pigments retained in a nylon filter (0.45 µm, 13 mm) from 30 mL of water. IT-SPME capillary was a fused silica capillary (10 cm length x 75 µm internal diameter, i.d.) with a coating of tetraethyl orthosilicato (TEOS), triethoximethylsilane (MTEOS) doped with SiO<sub>2</sub> nanoparticles (NPs) and an analytical column Zorbax 300SB-C<sub>18</sub> (50 mm x 75 µm i.d., 3.5 µm particle size) was used. The recovery obtained to chlorophyll a, chlorophyll <em>b</em> and β-carotene were 93 ± 8 %, 92 ± 7 % and 94 ± 4 %, respectively. The method shows good linearity in the range up to 300 µg L<sup>−1</sup> for chlorophyll a and β-carotene and up to 600 µg L<sup>−1</sup> for chlorophyll <em>b</em>. The achieved limits of detection (LODs) in samples were 0.1 µg L<sup>−1</sup> to chlorophyll a and β-carotene, and 0.2 µg L<sup>−1</sup> to chlorophyll <em>b</em>. Values of relative standard deviations (RSD) expressed in% between 2 and 3 were obtained. Pigments were successfully determined with a short analysis time and minimal residues in real water samples.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"8 ","pages":"Article 100093"},"PeriodicalIF":0.0,"publicationDate":"2023-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49759122","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Lourdes Ramos , Jose Manuel Herreros-Martínez , Belén Gómara , Valerie Pichon , Elefteria Psillakis
{"title":"The potential of new solvents and materials in the context of green analytical chemistry","authors":"Lourdes Ramos , Jose Manuel Herreros-Martínez , Belén Gómara , Valerie Pichon , Elefteria Psillakis","doi":"10.1016/j.sampre.2023.100096","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100096","url":null,"abstract":"","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"8 ","pages":"Article 100096"},"PeriodicalIF":0.0,"publicationDate":"2023-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49750836","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Neonicotinoids: An overview of the newest sample preparation procedures of environmental, biological and food matrices","authors":"Luca Ferrari, Andrea Speltini","doi":"10.1016/j.sampre.2023.100094","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100094","url":null,"abstract":"<div><p>An overview of the actual state-of-the-art sample treatment procedures for trace and ultra-trace determination of neonicotinoids (NQs) in environmental, food and biological samples is presented. Analytical procedures for NQs, sometimes together with their metabolites/by-products, and NQ-related new generation pesticides have been considered, focusing on sample preparation, which is essential in most cases due to both the complexity of the matrices and low concentrations of residual analytes. Different strategies have been practised for analytes extraction/preconcentration/cleanup, entailing various techniques as solid-liquid extraction (SLE), liquid-liquid extraction (LLE), offline and online solid-phase extraction (SPE), dispersive SPE (d-SPE), magnetic SPE (MSPE), solid-phase microextraction (SPME) and the quick, easy, cheap, effective, rugged and safe (QuEChERS) approach. New solid phases, including inorganic and carbon-based materials, have been prepared, also starting from “green” precursors, and successfully employed in the sample treatment step before hyphenated liquid chromatography or direct electrochemical detection. As well, new environmentally friendly solvents have been evaluated for LLE. The most recent studies (2022-present), around 50 papers, have been reviewed by matrix type, briefly described and commented concerning extraction efficiency, matrix effect, sensitivity, ease of application and sample throughput. Advantages and drawbacks were highlighted, as well as new achievements paving the way for further improvements.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"8 ","pages":"Article 100094"},"PeriodicalIF":0.0,"publicationDate":"2023-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49750631","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Emulsification liquid-liquid microextraction coupled with droplet digital image colorimetric detection for determination of rhodamine B in food and beverage samples","authors":"Niluh Indria Wardani , Waleed Alahmad , Hadi Tabani , Pakorn Varanusupakul","doi":"10.1016/j.sampre.2023.100091","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100091","url":null,"abstract":"<div><p>An analytical method combining fatty acid-emulsification liquid-liquid microextraction (FA-ELLME) with solidification of floating drops (SFD) and droplet digital image colorimetry (DDIC) was developed for the analysis of rhodamine B (RhB) in food and beverage samples. This work applied an emulsified amphiphilic fatty acid as an extracting solvent and a freezing procedure for extracting phase separation. A 7 mL sample volume adjusted to pH 5 was extracted with a drop of 35 μL of octanoic acid (0.5%v/v). The emulsification was initiated by shaking for 10 s followed by centrifugation for 5 min. The floating drops containing RhB were solidified in an ice bath, separated from the solution, defrosted, and dropped on the paper platform for DDIC analysis. The limit of detection (LOD) and limit of quantification (LOQ) were 1.8 μg L<sup>−1</sup> and 6.0 μg L<sup>−1</sup>, respectively. The linear range was 10 - 40 μg L<sup>−1</sup> (R<sup>2</sup> = 0.997). The method was applied to determine RhB in beverage, candy, jelly, and chili sauce samples. The relative recovery percentages (RR%) between 73% and 113% were achieved.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"8 ","pages":"Article 100091"},"PeriodicalIF":0.0,"publicationDate":"2023-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49759121","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Comparison of fragrance and flavor components in non-psilocybin and psilocybin mushrooms using vacuum-assisted headspace high-capacity solid-phase microextraction and gas chromatography–mass spectrometry","authors":"Shannon L. Thomas , Colton Myers , Kevin A. Schug","doi":"10.1016/j.sampre.2023.100090","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100090","url":null,"abstract":"<div><p>Vacuum-assisted headspace high capacity solid-phase microextraction (Vac-HS-HC-SPME) coupled with gas chromatography–mass spectrometry (GC–MS) was used to compare the volatile compounds that make up the volatile and semi-volatile components of five psilocybin mushrooms (<em>Psilocybe cubensis</em>), as well as three non-psilocybin mushroom species. Using an untargeted analysis, common volatiles detected consisted of acids, alcohols, aldehydes, ketones, and hydrocarbons. The initial comparison of Vac-HS-HC-SPME and HS-HC-SPME conditions showed 2 times increase in compound response as well as the detection of 8 additional compounds undetected by HS-HC-SPME. Compounds unique to psilocybin mushrooms were 2-methylbutanal, valeraldehyde, benzaldehyde, 3-octen-2-one, 2-methyl-dodecane, and 2‑butyl‑2-octenal. Compounds unique to non-psilocybin mushrooms were 2-methyl-pyrazine, 2,3-butanediol, butyric acid, butyrolactone, benzyl alcohol, 2-pyrrolidinone, and estragole. The commonly shared compound, 1-octen-3-ol, was shown to have a higher compound response among the psilocybin mushroom species.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"8 ","pages":"Article 100090"},"PeriodicalIF":0.0,"publicationDate":"2023-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49759351","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Determination of selenium in cereal and biofortified samples by ICP-OES using an alcohol-based deep eutectic solvent in digestion procedure","authors":"Masixole Sihlahla , Anele Mpupa , Marcin Sojka , Agnieszka Saeid , Philiswa Nosizo Nomngongo","doi":"10.1016/j.sampre.2023.100092","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100092","url":null,"abstract":"<div><p>The application of deep eutectic solvents (DESs) as green solvents in analytical chemistry has attracted increasing attention. The present study presents a simple, eco-friendly, and cost-effective approach for the extraction of selenium (Se) in food samples. The extraction method utilised alcohol-based DES and inductively coupled plasma optical emission spectrometry (ICP-OES) to determine total Se. Factors affecting the extraction procedure were optimised using the design of experiments. Using the optimal conditions, the limits of detection (LOD) and quantification (LOQ) and linearity of the developed method were 0.0011 µg Se/g, 0.0037 µg Se/g and 0.004–0.20 µg Se/g, respectively. The precision expressed as relative standard deviations (RSDs) was less than 10 %. The accuracy of the method was investigated using certified reference materials (IRMM 804 Rice Flour and NIST SRM 1567b wheat flour), and the results were in close agreement with the certified values (0.038 µg/g and 1.14 µg/g) with percentage recoveries ranging from 89.5 to 106 %. The interday ( %RSD) and Intraday ( %RSD) were 2.8–5.4 % and 4.3–5.9 %, respectively. The greenness of the method was assessed using NEMI, AES, and AGREE metrics tools. When comparing all these tools, they all qualified the proposed method as green.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"8 ","pages":"Article 100092"},"PeriodicalIF":0.0,"publicationDate":"2023-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49750573","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Waleed Alahmad , Shaymaa A. Mohamed , Ahmad Halabi
{"title":"Recent elaborations in electromembrane microextraction technique for preconcentration of chromium species: A mini-review","authors":"Waleed Alahmad , Shaymaa A. Mohamed , Ahmad Halabi","doi":"10.1016/j.sampre.2023.100097","DOIUrl":"https://doi.org/10.1016/j.sampre.2023.100097","url":null,"abstract":"<div><p>In recent years, electromembrane microextraction techniques have been used widely for the analysis of chromium species (trivalent and hexavalent chromium) in different environmental matrices. It is based on the electrokinetic migration across a membrane under the effect of an external electrical field between two aqueous phases. Trace analysis in complex matrices usually requires an effective sample preparation step to isolate, extract, and enrich the target analytes. Due to its distinctive qualities, including a high degree of enrichment factors, clean-up, and conformity with green chemistry principles, electromembrane microextraction techniques are among the methods for extracting chromium that have gained much attention in recent years. These techniques could be classified into two groups; electromembrane extraction (EME) which is based on using hydrophobic compounds (e.g., a few microliters of organic solvents) to separate the two aqueous solutions (donor and acceptor solutions), and gel electromembrane microextraction (G-EME) which is based on using a membrane made of biopolymers. In this review, the most recent advancements in EME and G-EME technologies for the extraction of chromium species in environmental samples in the last five years were summarized. Furthermore, the performance of the systems is evaluated in terms of their precision and accuracy, detection limits, and merits and drawbacks. Finally, future perspectives on these techniques were discussed.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"8 ","pages":"Article 100097"},"PeriodicalIF":0.0,"publicationDate":"2023-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49750185","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}