Advances in Sample Preparation最新文献

{"title":"Electric field-assisted dried blood spot sample preparation for analysis of steroids using LC–MS/MS","authors":"Ramisa Fariha,&nbsp;Emma Rothkopf,&nbsp;John Murphy,&nbsp;Nondi Walters,&nbsp;Oluwanifemi David Okoh,&nbsp;Nabil M. Lawandy,&nbsp;Anubhav Tripathi","doi":"10.1016/j.sampre.2024.100115","DOIUrl":"10.1016/j.sampre.2024.100115","url":null,"abstract":"<div><p>Despite being a minimally invasive sample source, dried blood spots (DBS) generally pose the challenge of efficient sample extraction for broad metabolomics applications. This is particularly true for the quantification of steroids using non-derivatized liquid chromatography tandem mass spectrometry assays. To address these limitations, we have demonstrated the use of electric field as a driver for sample preparation from DBS samples to simultaneously quantify testosterone (T), 17α-hydroxyprogesterone (17-OHP), progesterone (P), and cortisol (C), using both standard electroporation cuvettes, as well as a novel custom vertical electric field setup. Our findings, backed by computational modeling, show that a 10V DC application for 180 s can draw out twice the amount of the aforementioned steroids from both Whatman-903 and DMPK-C sample collection cards using our novel device when compared to standard solvent-based collection methods. This study not only introduces the use of electric field for sample preparation for metabolomics, but additionally introduces a novel device that eliminates the electric double layer effect in the process.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"10 ","pages":"Article 100115"},"PeriodicalIF":0.0,"publicationDate":"2024-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000147/pdfft?md5=1e87ac8cf644213ba412e595abca12e2&pid=1-s2.0-S2772582024000147-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141136737","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":"Enhancing biomarker detection in human serum for lung cancer diagnosis: Aqueous biphasic systems for simultaneous depletion of high-abundance proteins and efficient extraction of CYFRA 21–1","authors":"Marguerita E. Rosa,&nbsp;Maria S.M. Mendes,&nbsp;Diana C.V. Belchior,&nbsp;João A.P. Coutinho,&nbsp;Francisca A. e Silva,&nbsp;Mara G. Freire","doi":"10.1016/j.sampre.2024.100116","DOIUrl":"10.1016/j.sampre.2024.100116","url":null,"abstract":"<div><p>Analysing biomarkers in human serum could be used as an effective and less invasive approach for the diagnosis of lung cancer; however, biomarker detection reliability is highly limited due to matrix effects. Herein, aqueous biphasic systems (ABS) are studied as platforms for human serum pretreatment, allowing the simultaneous depletion of high abundant proteins and biomarker extraction. By using ABS varying the polyethylene glycol (PEG) molecular weight between 400 and 6000 g·mol⁻¹ and adopting phosphate buffer as the other phase-forming component, the depletion of the high abundance serum proteins immunoglobulin G (IgG) and human serum albumin (HSA) is induced at the ABS interphase, through precipitation, forming a three-phase partitioning system (ABS-TPP). Maximum depletion efficiencies of 99 % for IgG and 70 % for HSA were achieved in one step using PEG 1500-based ABS-TPP. On the other hand, lung cancer biomarkers, such as CYFRA 21–1, are extracted to the PEG-rich phase of the same ABS-TPP with recovery yields of 91 %. This work shows that a proper selection of the PEG molecular weight in the ABS composition leads to the efficient depletion of high-abundance proteins and extraction of cancer biomarkers from human serum, in a single step, confirming the potential of ABS for sample pretreatment to improve biomarker analysis.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"10 ","pages":"Article 100116"},"PeriodicalIF":0.0,"publicationDate":"2024-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000159/pdfft?md5=cc952288acd7046329196162d433f14a&pid=1-s2.0-S2772582024000159-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141138133","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":"Simple and accurate on-site quantitation of BTEX in atmospheric air using solid-phase microextraction and gas chromatography with photoionization detection","authors":"Tolkyn Kurmanbayeva,&nbsp;Bauyrzhan Bukenov,&nbsp;Zhansaya Rymzhanova,&nbsp;Nargiz Kazhkenova,&nbsp;Aibolat Imangabassov,&nbsp;Aruzhan Smail,&nbsp;Nurbi Karimkyzy,&nbsp;Bulat Kenessov","doi":"10.1016/j.sampre.2024.100117","DOIUrl":"10.1016/j.sampre.2024.100117","url":null,"abstract":"<div><p>This paper represents an improved method for on-site quantitation of benzene, toluene, ethylbenzene, and xylenes (BTEX) in atmospheric air using solid-phase microextraction (SPME) and portable gas chromatography with a split/splitless inlet and photoionization detector (GC-PID). The developed method includes air pumping to four replicate 250 mL gas sampling bulbs, three of which are extracted by 85 µm Carboxen/polydimethylsiloxane (Car/PDMS) coating at 40°C, while the last one is spiked with BTEX standard in nitrogen and extracted under the same conditions. Compared to other similar SPME-based methods, the developed method does not require a standard gas generator and traceable certified permeation tubes for instrument calibration.</p><p>The method was applied for on-site BTEX quantitation in air of Talgar, Almaty oblast, Kazakhstan in February and March 2024, at two different extraction times, among which 15 min was chosen as optimal because it provided sufficient detection limits of ethylbenzene, and xylenes. The on-site standard addition calibration allowed accurate BTEX quantitation. In February, only benzene (18.3 and 6.8 µg/m³) and toluene (15.7 and 8.5 µg/m³) were detected. In March samples, concentrations of benzene were 12.3 and 7.4 µg/m³, toluene - 23 and 5.4 µg/m³, ethylbenzene – 5.5 µg/m³ and not detected, <em>m</em>-/<em>p</em>-xylene - 3.6 and 2.1 µg/m³, <em>o</em>-xylene - 6.8 and 10.6 µg/m³. The LODs for benzene, toluene, ethylbenzene, <em>m</em>-/<em>p</em>-xylene, and <em>o</em>-xylene were 0.07, 0.3, 2, 0.8 and 2 µg/m³, respectively. The developed method can be recommended for quick and low-cost on-site quantification of BTEX in atmospheric air, particularly at remote locations.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"10 ","pages":"Article 100117"},"PeriodicalIF":0.0,"publicationDate":"2024-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000160/pdfft?md5=ae17d870cb15ac7c8196bd6f27484780&pid=1-s2.0-S2772582024000160-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141136595","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":"Perspective on sample preparation fundamentals","authors":"Martyna N. Wieczorek ,&nbsp;Wei Zhou ,&nbsp;Janusz Pawliszyn","doi":"10.1016/j.sampre.2024.100114","DOIUrl":"https://doi.org/10.1016/j.sampre.2024.100114","url":null,"abstract":"<div><p>The primary objective of this contribution is to offer insights into fundamentals associated with typical sample preparation, facilitating rational design of new analytical technologies and effective optimization of existing techniques. Sample preparation stands a pivotal stage in the analytical process. Unfortunately, the optimization of associated parameters often relies on trial and error rather than systematic scientific methodologies. If an extraction method provides good recovery of spikes of standards, it is assumed that it works well and no further consideration is given to the underlying principles driving its performance. In the realm of sample preparation, the fundamentals of method optimization are not accorded the same significance as in other technologies, such as chromatography or mass spectrometry. Consequently, the fundamentals of sample preparation are typically overlooked in analytical chemistry curricula.</p><p>A notable impediment to progress in the sample preparation area is underdeveloped understanding of the fundamentals of extraction, particularly when dealing with natural, often complex samples, where native analyte-matrix interaction is different compared to spikes. This stands in contrast to the physiochemically simpler systems employed in separation and quantification steps, such as chromatography and mass spectrometry.</p><p>A careful consideration of the underlying principles of sampling and sample preparation can lead to the creation of more efficient and environmentally friendly technologies. Embracing these principles aligns with global shift towards more sustainable future, challenging the perception that sample preparation is solely an artistic endeavour and highlighting its potential as a scientifically grounded discipline.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"10 ","pages":"Article 100114"},"PeriodicalIF":0.0,"publicationDate":"2024-04-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000135/pdfft?md5=29e0aa560ef39e2836c0fa2e057b3981&pid=1-s2.0-S2772582024000135-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140536252","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":"Recent cutting-edge approaches to the integration of solid-liquid extraction with deep eutectic solvents: Toward a greener procedure for biomass valorization","authors":"Niluh Indria Wardani ,&nbsp;Thidarat Samkumpim ,&nbsp;Waleed Alahmad ,&nbsp;Andrew William King ,&nbsp;Pakorn Varanusupakul ,&nbsp;Andrey Shishov ,&nbsp;Noorfatimah Yahaya ,&nbsp;Nur Nadhirah Mohamad Zain","doi":"10.1016/j.sampre.2024.100113","DOIUrl":"https://doi.org/10.1016/j.sampre.2024.100113","url":null,"abstract":"<div><p>As the global demand for sustainable and renewable resources intensifies, there is an imperative to explore innovative technologies for biomass valorization. This review delves into a promising avenue, providing an overview of green approaches that combine solid-liquid extraction (SLE) with a type of solvent known as deep eutectic solvents (DESs) in a synergistic manner. SLE, a conventional method for isolating bioactive compounds from biomass, is recognized for its effectiveness in sample preparation. However, it often involves the use of environmentally harmful solvents. Subsequently, DESs have emerged as an eco-friendly alternative to traditional solvents. Composed of naturally occurring and benign components, these DESs exhibit unique properties that render them suitable for various extraction processes. The integration of SLE with DESs introduces a novel approach to biomass valorization. This review explores the synergistic effects between SLE and DESs to optimize extraction yields, improve selectivity, and reduce overall energy consumption. Furthermore, the nature of DESs aligns with the principles of green chemistry, positioning them as a sustainable alternative to traditional solvents.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"10 ","pages":"Article 100113"},"PeriodicalIF":0.0,"publicationDate":"2024-03-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000123/pdfft?md5=dbc23c7eac0f6fedd1940ef8f67b24b3&pid=1-s2.0-S2772582024000123-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140342107","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":"Advances in sample preparation for volatile profiling of plant proteins: Fundamentals and future perspectives","authors":"Wellington da Silva Oliveira,&nbsp;Igor Shepelev,&nbsp;Fernanda F.G. Dias,&nbsp;Gary A. Reineccius","doi":"10.1016/j.sampre.2024.100111","DOIUrl":"10.1016/j.sampre.2024.100111","url":null,"abstract":"<div><p>Due to the increasing world population and consumer desire for sustainable and nutritious protein sources, the food industry is currently experiencing tremendous pressure to develop innovative, sensorially acceptable, health-promoting plant-based products. Plant proteins, specifically pulse proteins arise as a healthy and sustainable protein source for food applications. However, the use of pulse protein is challenged by its intrinsic undesirable aroma often described as beany, grassy, and green. These off notes can be inherent, i.e. generated from plant metabolism, or produced during processing and/or storage and encompass a broad variety of chemical classes. Since aroma plays a major role in consumer acceptance and eating habits and due to its chemical complexity, proper analytical methods must be used for its assessment. Considering that the effectiveness of an analytical method is significantly influenced by its sample preparation step, this review focuses on sample preparation techniques for monitoring the volatile profile of pulse proteins, their advantages, and disadvantages, while concurrently highlighting the potential of novel technologies for advancing this critical application.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"10 ","pages":"Article 100111"},"PeriodicalIF":0.0,"publicationDate":"2024-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S277258202400010X/pdfft?md5=f42c49068959ead6a21a9b61a55853f7&pid=1-s2.0-S277258202400010X-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140271118","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":"Development of Dry-herb vaporizer-assisted solid-phase Microextraction for the analysis of volatile Organic compounds","authors":"A K M Ahsan Ahmed,&nbsp;Douglas E. Raynie","doi":"10.1016/j.sampre.2024.100112","DOIUrl":"https://doi.org/10.1016/j.sampre.2024.100112","url":null,"abstract":"<div><p>Solid-phase microextraction (SPME) is a simple, efficient, and solvent-free technique. It integrates the steps of traditional liquid-liquid extraction, i.e., sampling, extraction, concentration, derivatization, in a single step. It is easy, combining capability with gas chromatography (GC), liquid chromatography (LC), and mass spectrometry (MS), which makes this method fast, reliable, and sensitive. SPME method is often associated with extraction at elevated temperature, since increasing temperature may positively affect extraction by increasing the analyte volatility, diffusion, and extraction rate. In this work, a dry-herb vaporizer (vaping pen) was used as a sample heating device for direct desorption of volatile analytes into the headspace of the device. The extraction was performed by sorbing analytes from their gas phase in the headspace of the vape onto a SPME fiber followed by desorption in the injection port for GC–MS characterization. Compounds from horseradish, cinnamon, and gasoline-spiked soil samples were analyzed. The samples were also analyzed by conventional headspace SPME-GC–MS. The results from both methods were compared. The methods produce comparable results in terms of extracted compounds and relative area percentages, however, the dry-herb vaporizer had improved sensitivity.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"10 ","pages":"Article 100112"},"PeriodicalIF":0.0,"publicationDate":"2024-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000111/pdfft?md5=0c98a404a2a7657445ab73f884a14fb5&pid=1-s2.0-S2772582024000111-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140163657","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":"Assessing the potentialities of an easy-to-use sample treatment strategy: Multivariate investigation on “Moka extraction” of typical ingredients from dietary supplements","authors":"Matteo Baglietto,&nbsp;Barbara Benedetti,&nbsp;Marina Di Carro,&nbsp;Emanuele Magi","doi":"10.1016/j.sampre.2024.100110","DOIUrl":"https://doi.org/10.1016/j.sampre.2024.100110","url":null,"abstract":"<div><p>Mr. Bialetti invented Moka in 1933 and it still represents the most common way to prepare coffee at home. The process through which Mokas extract components from the ground coffee is a solid-liquid extraction which occurs at high pressure and temperature. These features are desirable in simple sample treatment strategies, since they allow good extraction efficiencies in a short time. Herein, for the first time, Moka-pot extraction was considered as an alternative processing protocol to extract polar compounds from dietary supplements. The effect of four experimental variables on extraction efficiency was evaluated through a fractional factorial design of experiments applied to a pooled matrix. In particular, solvent pH and its content of organic modifier, heating temperature and sample mass (reflecting the ratio to the amount of solvent which has to be kept fixed due to practical needs) were considered. The performances of the best conditions were then validated by determining recoveries (between 52 and 134 %, except for acetylsalicylic acid) and matrix effects (resulting always negligible or moderate at 100-fold dilution) of a spiked matrix which did not present any of the target analytes. They were finally applied to real samples, allowing to quantify some compounds, including artificial sweeteners, methylxanthines and taurine. Results were then compared with the quantities declared on the labels and those obtained with a Salt-Assisted Liquid-Liquid Extraction (SALLE), previously developed. Interestingly, the two methods were comparable for most compounds, but Moka extraction allowed to quantify taurine, which was not recovered with the SALLE. This promising result encourages further work to extend the use of the simple Moka device to other analytes and further matrices.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"10 ","pages":"Article 100110"},"PeriodicalIF":0.0,"publicationDate":"2024-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000093/pdfft?md5=6e6e252f8609bf70fc14f3ca6793fccd&pid=1-s2.0-S2772582024000093-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140134961","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":"Effects of thermal treatment on quality of biosimilar and originator monoclonal antibodies","authors":"Yiğit Erdemgil ,&nbsp;Merve Çelik Yamacı ,&nbsp;Ceren Pamukcu ,&nbsp;Fulya Ünalp ,&nbsp;Zeynep Zülfiye Yıldırım Keleş ,&nbsp;Ahmet Emin Atik ,&nbsp;Muhittin Abdulkadir Serdar","doi":"10.1016/j.sampre.2024.100109","DOIUrl":"https://doi.org/10.1016/j.sampre.2024.100109","url":null,"abstract":"<div><p>Investigating products under stress conditions provides valuable information for assessing stability, biosimilarity, and degradation behaviors during monoclonal antibody (mAb) development. Proper sample preparation is crucial for accurately evaluating the biosimilarity and effects of stress conditions in comparability assessment, where these studies guide biosimilar mAb development steps. Enzymatic and chemical treatments applied during sample preparation of mAbs generally require treatment of samples in temperatures higher than the storage temperatures of antibodies.</p><p>In this study, samples of a TNF-α inhibitor IgG1 biosimilar (BIO) and its originator (OR) were treated for 7 days at commonly used temperatures during sample preparation. Alterations in the intact IgG, size variants, charge variants, binding kinetics, and post-translational modifications (PTMs) were investigated with CE-SDS, SE-UPLC, icIEF, SPR, and LC-MS/MS, respectively. Samples treated at 50 °C exhibited significant degradation, while minor differences were observed in samples treated at 37 °C. Monomer and intact IgG levels were decreased to levels below 97 % and 94 %, respectively, after 7 days of thermal treatment at 50 °C for both BIO and OR samples. Similar rates of degradation were observed between the treated biosimilar and originator samples. The percent monomer degradation rate between the biosimilar and the originators was similar at 50 °C (<em>p</em> = 0.32). Thermal treatment increased acidic variant levels in the products of the BIO (23.10 %) and OR (23.16 %). During post-translational modification monitoring, an increase in pyroglutamic acid formation and a decrease in C-terminal lysine were observed after thermal treatments. Acidic variant alterations were associated with asparagine deamidation and N-terminal pyroglutamic acid formation. Post-translational modifications were mainly located at the Fc domain, with methionine oxidation and asparagine deamidation as the main modifications occurring at the Fab domain.</p><p>In conclusion, these results revealed that prolonged thermal treatment under elevated temperatures induces molecular alterations, thereby facilitating the degradation of IgG1. In addition, our findings indicate that both BIO and OR lots exhibit similar degradation profiles when subjected to thermal treatments.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"10 ","pages":"Article 100109"},"PeriodicalIF":0.0,"publicationDate":"2024-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000081/pdfft?md5=f2fff2cf782d7b7e6bb834cc47657b18&pid=1-s2.0-S2772582024000081-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140141792","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":"Carbon nanotubes in high internal phase emulsion polymer composite for packed-cartridge micro-solid-phase extraction of fluoroquinolones in urine","authors":"Francesca Merlo ,&nbsp;Francesca Colucci ,&nbsp;Giulia De Soricellis ,&nbsp;Francesca Rinaldi ,&nbsp;Enrica Calleri ,&nbsp;Antonella Profumo ,&nbsp;Andrea Speltini","doi":"10.1016/j.sampre.2024.100103","DOIUrl":"10.1016/j.sampre.2024.100103","url":null,"abstract":"<div><p>Aim of this study stands in the evaluation of a carbon nanotubes-based polymerized high internal phase emulsion composite (CNT/polyHIPE) as sorptive phase in biological sample preparation. A micro-solid-phase extraction procedure (µSPE) was developed for trace fluoroquinolone (FQ) antimicrobials, namely Ciprofloxacin, Levofloxacin, Lomefloxacin, Moxifloxacin, Norfloxacin and Sparfloxacin, in human urine samples. PolyHIPEs modified by incorporation of different concentrations of nanotubes (0.2–0.8 wt %) were one-pot synthesized and applied in the packed-cartridge setting. The sorption affinity for the drugs was investigated in tap water and buffered aqueous solutions, demonstrating the key role of the nanotubes embedded in the polymer. The 0.5 wt % CNT composite was selected to develop a straightforward µSPE procedure directly in raw urine (1 mL sample), followed by HPLC-MS/MS. Targets were retained on the sorbent at near neutral pH and, after an aqueous washing (0.1 % v/v formic acid), eluted in a single-step with 4 % v/v ammonia aqueous solution (15 % v/v acetonitrile), thus combining extraction and clean-up. The method allowed accurate quantification of FQs, as evidenced by the recoveries (74–116 %, <em>n</em> <em>=</em> <em>3</em>) obtained on blank pooled urine samples spiked with 40, 75, 150 µg L⁻¹, accompanied by good inter-day precision (RSD &lt; 14 %, <em>n</em> <em>=</em> <em>3</em>). To confirm the applicability of the analytical method, some real-life blind samples were processed as a proof of concept.</p></div>","PeriodicalId":100052,"journal":{"name":"Advances in Sample Preparation","volume":"9 ","pages":"Article 100103"},"PeriodicalIF":0.0,"publicationDate":"2024-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2772582024000020/pdfft?md5=98be2f4f951125d5a73daa5c783e09ed&pid=1-s2.0-S2772582024000020-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139632388","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}