Analytical science advances最新文献

{"title":"Current PAT Landscape in the Downstream Processing of Biopharmaceuticals","authors":"Pavithra Sathiyapriyan,&nbsp;Shatanik Mukherjee,&nbsp;Thomas Vogel,&nbsp;Lars-Oliver Essen,&nbsp;David Boerema,&nbsp;Martin Vey,&nbsp;Uwe Kalina","doi":"10.1002/ansa.70013","DOIUrl":"https://doi.org/10.1002/ansa.70013","url":null,"abstract":"<p>Protein-based therapeutics have revolutionized modern medicine, addressing complex diseases with unprecedented specificity and efficacy. The rising demand for biologics has driven the evolution of biomanufacturing practices to ensure consistent quality and operational efficiency. Traditional batch testing, with its inherent limitations, is being replaced by quality by design (QbD) frameworks and process analytical technology (PAT). PAT facilitates real-time monitoring and control by integrating advanced analytical tools and data-driven methodologies to optimize downstream processing (DSP). This review highlights the recent advancements in PAT tools, including spectroscopy, chromatography and biosensors. Spectroscopic techniques provide rapid, non-invasive measurements, while biosensors offer high specificity for monitoring critical quality attributes. Additionally, the integration of chemometric modelling and digital twins enables predictive analytics and enhances process control, paving the way for real-time release (RTR) of the product. Despite challenges in regulatory compliance and technology integration, innovations in automation and machine learning are bridging these gaps, accelerating the transition to intelligent manufacturing systems. This article provides a comprehensive evaluation of emerging analytical technologies and strategic insights into their integration, aiming to support the biopharmaceutical industry's shift towards robust, continuous and adaptive manufacturing paradigms.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"6 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2025-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/ansa.70013","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144171819","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":"Waste PET Plastic-Derived UIO-66(Zr)-MOF Adsorbent for Dispersive Solid Phase Extraction and Removal of Penicillin Antibiotics Water Systems","authors":"Inga Skans,&nbsp;Mthokozisi Mnguni,&nbsp;Philiswa Nosizo Nomngongo","doi":"10.1002/ansa.70023","DOIUrl":"https://doi.org/10.1002/ansa.70023","url":null,"abstract":"<p>The extensive use or misuse of broad-spectrum antibiotics such as penicillins and their existence in various water bodies is still one of increasing global concern due to their persistent nature, which could potentially lead to human health and environmental risks. Recycling or upcycling plastic waste to value-added products such as metal-organic frameworks (MOF) to solve other environmental problems, such as water pollution, has received more attention. As a result, UiO-66(Zr)-MOF derived from recycled waste PET bottles (PET-derived UiO-66(Zr)-MOF) was investigated for enrichment and removal of amoxicillin (AMX) and penicillin G (PNG) in water bodies. The synthesised adsorbent was characterised using different analytical characterisation techniques. UiO-66(Zr)-MOF produced the maximum adsorption capacities of 139 and 147 mg/g for AMX and PNG, respectively. Freundlich and pseudo-second-order kinetics models best explained the adsorption process. The dispersive micro-solid phase extraction (D-μ-SPE) of the target analytes was performed using a high-performance liquid chromatography-diode array detector (HPLC-DAD). The effectiveness of the developed method was confirmed by its remarkable analytical performances, such as limits of detection (0.19–0.21 µg/L) while the linear range was 0.6–1000 µg/L. The feasibility and applicability of the validated UiO-66(Zr)-MOF-D-μ-SPE/HPLC-DAD method were confirmed by applying it in real water analysis. The AMX and PNG were detected in wastewater samples in the ranges of 1.51–4.71 µg/L and 0.195–1.19 µg/L for influent and effluent. The spike recoveries ranged from 89.9% to 101%, while the precision (intraday and interday) of the method was less than 5%.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"6 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2025-05-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/ansa.70023","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144135643","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 Suspended Droplet Microextraction Method for Spectrophotometric Determination of Serum Iron","authors":"Aruna Jyothi Kora,&nbsp;K. Madhavi,&nbsp;N. N. Meeravali","doi":"10.1002/ansa.70022","DOIUrl":"https://doi.org/10.1002/ansa.70022","url":null,"abstract":"<p>A facile, selective and sensitive method was devised for the Fe³⁺ quantification in low volume samples, such as bovine serum based on suspended droplet microextraction (SDME). Various process parameters such as concentrations of acid (1.5% hydrochloric acid), complexing agent (0.7% ammonium thiocyanate), quaternary ammonium salt (0.2% Aliquat 336) and extracting solvent (500 µL octanol) were optimised. Ammonium thiocyanate forms water soluble, red coloured, anionic ferric thiocyanate complex [Fe(SCN)₆]³⁻ with Fe³⁺ ions released from the iron–protein complex under an acidic medium. Negatively charged [Fe(SCN)₆]³⁻ complex forms hydrophobic ion associate Fe(SCN)₆³⁻–Aliquat 336₃³⁺ with hydrophilic NH₄⁺ head groups of Aliquat 336 and drives out the formed micelle from aqueous solution along with the iron complex. After stirring, ion associate bonded micelles are separated into a hanging micro droplet of octanol. Red coloured ferric thiocyanate complex in a suspended droplet is solubilised in methanol and Fe³⁺ concentration in serum samples is obtained by recording the spectrophotometric absorbance at 505 nm. The recoveries ranged from 96.2%–98.8% with relative standard deviation (RSD) (%) values from 1.4% to 5.0% at 100–400 ng/mL confirming interference free quantification at optimised conditions. The developed method was linear over the range of 20–1000 ng/mL of Fe³⁺ with a limit of detection of 2.4 ng/mL for the serum matrix. The developed method is applied to various bovine serum samples and Fe³⁺ concentration values ranged from 62.7 to 1582.5 ng/mL. The obtained values were in accordance with the results obtained from the electrothermal atomic absorption spectrometry at 99% confidence level using <i>t</i>-test indicating the accuracy of the developed method. The proposed procedure offers various advantages such as enhanced sensitivity of the spectrophotometer towards iron determination, low-cost complexing agent, low sample volume, metal and biological interference free, simplicity and selectivity. Thus, the developed method can be an alternative to the routine spectrophotometric analysis of low volume samples such as serum and other biological fluids.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"6 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/ansa.70022","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143950026","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":"The Dark Metabolome/Lipidome and In-Source Fragmentation","authors":"Winnie Uritboonthai,&nbsp;Linh Hoang,&nbsp;Aries Aisporna,&nbsp;Martin Giera,&nbsp;Gary Siuzdak","doi":"10.1002/ansa.70012","DOIUrl":"https://doi.org/10.1002/ansa.70012","url":null,"abstract":"&lt;p&gt;To the editor,&lt;/p&gt;&lt;p&gt;Tandem mass spectrometry (MS/MS) is valued for its ability to facilitate molecular identification and deliver highly consistent data across a wide range of mass spectrometry platforms. Distinct from MS/MS is the fragmentation that occurs during electrospray ionization (ESI), commonly referred to as in-source fragmentation (ISF) (Figure 1). ISF was first observed in the 1950s with electron ionization and has been recognized as an inherent yet often overlooked feature of the ESI process, albeit less prevalent than with electron ionization. Recently, ISF has been associated with the overrepresentation of peaks in liquid chromatography mass spectrometry (LC/MS) data, where it accounts for the majority of observed unfiltered peaks [&lt;span&gt;1&lt;/span&gt;]. Due to its overrepresentation in LC/MS data, and the subsequent inability to identify the molecules associated with these peaks using MS/MS data, ISF has been linked to the so-called “dark metabolome” [&lt;span&gt;2, 3&lt;/span&gt;] (also encompassing the lipidome), a term used to describe uncharacterized molecular species in metabolomics and lipidomics. This association [&lt;span&gt;1&lt;/span&gt;] was determined by an examination of MS/MS data acquired at 0 eV collision energy from METLIN's extensive library of over 931,000 molecular standards. However, while the similarity of ISF and MS/MS at 0 eV data has been described in previous studies [&lt;span&gt;1, 4&lt;/span&gt;–&lt;span&gt;6&lt;/span&gt;], it has yet to be directly established that they correlate with each other. We explored the consistency between MS/MS (0 eV) data and ISF across various molecular species to assess whether mining METLIN's MS/MS (0 eV) data—comprising over 931,000 molecular standards—can effectively link ISF to the dark metabolome and lipidome.&lt;/p&gt;&lt;p&gt;Liquid chromatography-tandem mass spectrometry (LC-MS/MS) with ESI has become a cornerstone in metabolomics, lipidomics, and clinical analysis due to its accuracy in identifying small molecules within complex biological matrices. With LC-MS/MS, after ionization occurs in the ESI source, charged molecules are directed into a collision cell where they undergo fragmentation for structural analysis. This procedure is typically repeated for all charged analytes present in a sample. However, despite its utility, this method has revealed an unexpectedly vast array of spectral features associated with the “dark metabolome.” However, given the limited number of protein-coding genes [&lt;span&gt;7, 8&lt;/span&gt;] with only a fraction producing enzymes, the chemical diversity [&lt;span&gt;3, 9, 10&lt;/span&gt;] detected through LC-MS/MS—potentially hundreds of thousands or even millions of metabolites—far exceeds biological expectations. Current estimates suggest that less than 2% of observed LC-MS/MS spectra can be annotated, a potentially broad spectrum of unknown compounds [&lt;span&gt;3&lt;/span&gt;]. Recent research [&lt;span&gt;1&lt;/span&gt;] using the METLIN database and its data at 0 eV has shed light on this discrepancy, and much of the perceived compl","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"6 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/ansa.70012","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143950025","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":"Comparison Between a New PSA Assay With the Well-Established Beckman Coulter Immunoassay: A Preliminary Report","authors":"Evelina La Civita,&nbsp;Mariano Fiorenza,&nbsp;Giuseppe Jannuzzi,&nbsp;Carmela Polito,&nbsp;Rosa Sirica,&nbsp;Gianluigi Carbone,&nbsp;Domenica Sorvillo,&nbsp;Aniello Saviano,&nbsp;Matteo Ferro,&nbsp;Daniela Terracciano","doi":"10.1002/ansa.70017","DOIUrl":"https://doi.org/10.1002/ansa.70017","url":null,"abstract":"<p>Prostate-specific antigen (PSA) is a critical biomarker for prostate cancer (PCa) patient clinical management. In this study, we sought to compare three different immunoassays (CLIA): Beckman Coulter Access Hybritech (PSA-B) (reference method), Immulite 2000 PSA (PSA-I) and the newly introduced Atellica IM PSA assay (PSA-A). We selected serum samples from our routine clinical testing at University Hospital Federico II between April and May 2024 from 104 men with a median age of 66 years (interquartile range = 57–74). Total PSA was determined using three different assays: PSA-B, PSA-A and PSA-I. A significant correlation between PSA-B and PSA-I assays was found for samples in the overall population (Spearman <i>r</i> (<i>ρ</i>) = 0.99, <i>p</i> &lt; 0.0001). PSA-I displayed a strong correlation with PSA-B for values below 2 ng/mL (<i>ρ</i> = 0.98, <i>p</i> &lt; 0.0001), for values between 2 and 10 ng/mL (<i>ρ</i> = 0.97, <i>p</i> &lt; 0.0001) and for values above 10 ng/mL (<i>ρ</i> = 0.77, <i>p</i> &lt; 0.0001). A significant positive correlation was found between PSA-B and PSA-A in the overall population (<i>ρ</i> = 0.97, <i>p</i> &lt; 0.0001) and in stratified analyses between PSA-A and PSA-B for values below 2 ng/mL (<i>ρ</i> = 0.86, <i>p</i> &lt; 0.0001), from 2 ng/mL to 10 ng/mL (<i>ρ</i> = 0.93, <i>p</i> &lt; 0.0001) and above 10 ng/mL (<i>ρ</i> = 0.77, <i>p</i> &lt; 0.0001). Although both PSA-I and PSA-A demonstrated a significant positive correlation with PSA-B, PSA-I displayed a significantly better correlation with PSA-B than PSA-A in samples with PSA below 2 ng/mL.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"6 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2025-05-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/ansa.70017","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143950024","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":"Release Monitoring and Detection of Formulated Solid Nanoparticle–Conjugated Nicotine in Blood and Urine Using Electrochemical Technique","authors":"Blessing Wisdom Ike,&nbsp;Joshua C. Nwabuife,&nbsp;John Alake,&nbsp;Darko Kwabena Adu,&nbsp;Lungelo Miya,&nbsp;Ruchika Chauhan,&nbsp;Zondi Nate,&nbsp;Rajshekhar Karpoormath,&nbsp;Mbuso Faya","doi":"10.1002/ansa.70018","DOIUrl":"https://doi.org/10.1002/ansa.70018","url":null,"abstract":"<p>Tobacco (nicotine) has been reported as one of the worst global public health pandemics in history, claiming about 8 million lives annually. According to the World Health Organisation (WHO), nicotine accounts for about 7 million deaths of firsthand users and over 1.3 million morbidities of secondhand users. Furthermore, smokeless tobacco products have been linked to more than 300 million morbidities, including chronic kidney illnesses. On the basis of this trend, a possible increase of over 100% in mortality rate and a state of emergency have been predicted from now till 2050. However, electrochemical analysis has demonstrated cost-effective and easily synthesised sensors as a timely alternative for the rapid analysis and quantification of nicotine in diverse products. A carbon-based silver sensor was fabricated and characterised by energy-dispersive x-ray (EDX) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), direct light scattering (DLS), and x-ray diffraction (XRD). Herein, we report the first electrochemical detection, release monitoring and quantification of conjugated nicotine. The sensor showed a significant sensitivity, specificity and discriminating power with a detection and quantification limit of 2.283 × 10⁻⁹ and 0.761 × 10⁻⁸ M, respectively. An average recovery rate of 96.26% was recorded. The applicability of the modified electrode was examined in human urine and serum. The research showed the potential of this method for monitoring doping and nicotine release, as well as for diagnostic and quality control purposes.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"6 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2025-05-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/ansa.70018","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143932381","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":"A New Mixed Biased Estimator for Ill-Conditioning Challenges in Linear Regression Model With Chemometrics Applications","authors":"Muhammad Amin,&nbsp;Sadiah M. A. Aljeddani,&nbsp;Muhammad Nauman Akram,&nbsp;Sajida Yasmeen","doi":"10.1002/ansa.70020","DOIUrl":"https://doi.org/10.1002/ansa.70020","url":null,"abstract":"<p>In linear regression models, the ordinary least squares (OLS) method is used to estimate the unknown regression coefficients. However, the OLS estimator may provide unreliable estimates in non-orthogonal models. This article introduces a novel mixed-biased estimator to address the challenges posed by the non-orthogonal model. The proposed estimator is derived through a combination of two estimators, namely, the Stein and ridge estimators. The theoretical properties of the proposed estimator are discussed. Moreover, we suggest estimation methods to estimate the value of the shrinkage parameters for the proposed estimator. We compare the performance of the proposed estimator with the Stein estimator, the ridge estimator with standard and two best ridge parameters and the ordinary least square estimator. This evaluation is based on the mean squared error performance criterion, using both a simulation study and two practical applications related to cement and crock datasets. The simulation study and applications results show that the proposed estimator performs better than the other considered estimators.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"6 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2025-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/ansa.70020","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143930514","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":"Mini Review: Highlight of Recent Advances and Applications of MALDI Mass Spectrometry Imaging in 2024","authors":"Yuen Tung Ngai,&nbsp;Darren Lau,&nbsp;Parul Mittal,&nbsp;Peter Hoffmann","doi":"10.1002/ansa.70016","DOIUrl":"https://doi.org/10.1002/ansa.70016","url":null,"abstract":"<p>Matrix-assisted laser desorption/ionisation mass spectrometry imaging (MALDI-MSI) is an emerging imaging tool that allows visualisation of hundreds of analytes unbiasedly in a single experiment. This paper highlights the adaptations of MALDI-MSI in different context in 2024, such as clinical diagnostic, pharmacology, forensics applications, plant metabolism and biology. Challenges and advancements were also discussed regarding sample preparation, instrumentations, data analysis, and integration of machine learning in the trend of single cell resolution and multi-omics. There are still rooms for improvements in sensitivity, spatial resolution, acquisition algorithm and data integration across multi-omics data to enable MALDI-MSI at subcellular level.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"6 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2025-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/ansa.70016","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143930512","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":"Efficient Nonenzymatic Electrochemical Detection of Glucose Using CuO Nanoparticles@CNT-Wrapped Graphene Oxide Composite Electrode","authors":"Amina Khalid,&nbsp;Rizwan Shoukat,&nbsp;Abid Ali,&nbsp;Salih Akyürekli,&nbsp;Arfaa Sajid,&nbsp;Muhammad Adeel Asghar,&nbsp;Qaisar Manzoor,&nbsp;Arif Nazir,&nbsp;Norah Alsadun,&nbsp;Amel Y. Ahmed","doi":"10.1002/ansa.70019","DOIUrl":"https://doi.org/10.1002/ansa.70019","url":null,"abstract":"<p>A highly sensitive and stable nonenzymatic glucose biosensor has been developed via composite materials composed of CuO and graphene oxide (GO)/carbon nanotube (CNT) nanohybrid (CuO/GO/CNTs). Copper oxide nanoparticle(NP)-modified CNTs were stacked via graphene sheets and synthesized through hydrothermal method, providing a larger surface area with boosted catalytic activity for efficient mass and electron passage, respectively. Scanning electron microscopy (SEM) and energy-dispersive x-ray (EDX) spectroscopy have been used to investigate the morphology and composition of as-prepared nanohybrids, whereas x-ray diffraction (XRD) patterns provide information about the crystal structure and lattice parameters. Fabricated nanohybrid was used as electrode material to develop the nonenzymatic glucose biosensor, which exhibited better performance with a linear dynamic range from 0.06 to 0.74 mM, a high sensitivity of 328 mA mM⁻¹ cm⁻² and a low detection limit of up to 0.033 mM with a fast response time of 2 s. Although the stability and reusability of the fabricated electrode have been tested. The limit of detection was determined by using the traditional formula LOD = (SNR × <i>σ</i>)/Slope. The outcomes recommend the synthesized novel structured nanohybrid as a promising material possessing significant impact for flexible and wearable biosensing applications.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"6 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2025-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/ansa.70019","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143930513","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":"Application of Iron Oxide Magnetic Nanoparticles Modified by Superhydrophobic Cellulose as a Sorbent for Solid-Phase Extraction of Fat-Soluble Vitamins","authors":"Fariborz Momenbeik,&nbsp;Arezoo Khatam","doi":"10.1002/ansa.70015","DOIUrl":"https://doi.org/10.1002/ansa.70015","url":null,"abstract":"<p>Superhydrophobic cellulose-coated magnetic nanoparticles (SCCMNPs) were synthesized and applied as an advanced solid-phase extraction (SPE) sorbent for the simultaneous extraction of fat-soluble vitamins (FSVs) (A, E and D₃). These modified nanoparticles (NPs) improve extraction efficiency and reduce process time through magnetic separation. The cellulose coating, further modified with stearoyl chloride, enhances sorbent stability and specificity, providing strong hydrophobic interactions while preventing NP aggregation. Extracted vitamins were quantified by high-performance liquid chromatography. Optimization of coating materials revealed that 1.0000 g cellulose and 1.00 mL stearoyl chloride per 1.0000 g magnetic NPs (MNPs) were optimal. The NPs were characterized using Fourier-transform infrared spectroscopy, alternating gradient force magnetometry, dynamic light scattering and zeta potential measurements. Optimized extraction conditions included 50.0 mg sorbent, 10.00 mL sample solution (pH = 5.0), 250 µL tetrahydrofuran as the desorption solvent and 1.5-min sorption/desorption times. Calibration curves exhibited excellent linearity (<i>R</i>² ≥ 0.999), with a dynamic linear range of 2.4 × 10¹–1.0 × 10³ µg/L, limits of detection ≤8.6 µg/L, repeatability (%relative standard deviation [RSD] ≤ 4.6) and accuracy (recovery ≥79.60%). This is the first report demonstrating the application of stearoyl-modified cellulose in SPE, enabling rapid, solvent-efficient and highly selective vitamin extraction. The method provides a sustainable, cost-effective and high-performance alternative to conventional SPE, achieving efficient recovery with minimal sorbent amount, attributed to its optimized hydrophobicity from the affordable cellulose support. The application of this method in extracting FSVs from pharmaceutical formulations highlights these NPs as a promising next-generation SPE sorbent, offering an efficient, selective and environmentally benign solution.</p>","PeriodicalId":93411,"journal":{"name":"Analytical science advances","volume":"6 1","pages":""},"PeriodicalIF":3.0,"publicationDate":"2025-05-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/ansa.70015","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143909096","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}