Journal of chromatography open最新文献

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Optimization of the ionic liquid-based dispersive liquid–liquid microextraction combined with high-performance liquid chromatography coupled with diode array detection for the determination of multiclass pesticide residues in water samples 离子液体分散液液微萃取-高效液相色谱-二极管阵列检测联合检测水样中多类农药残留的优化研究
Journal of chromatography open Pub Date : 2025-06-05 DOI: 10.1016/j.jcoa.2025.100231
Bezuayehu Tadesse Negussie , Simiso Dube , Mathew Muzi Nindi , Asmamaw Tesfaw
{"title":"Optimization of the ionic liquid-based dispersive liquid–liquid microextraction combined with high-performance liquid chromatography coupled with diode array detection for the determination of multiclass pesticide residues in water samples","authors":"Bezuayehu Tadesse Negussie ,&nbsp;Simiso Dube ,&nbsp;Mathew Muzi Nindi ,&nbsp;Asmamaw Tesfaw","doi":"10.1016/j.jcoa.2025.100231","DOIUrl":"10.1016/j.jcoa.2025.100231","url":null,"abstract":"<div><div>An expeditious and effective analytical methodology, predicated on ionic liquid-based dispersive liquid–liquid microextraction (IL-DLLME) integrated with high-performance liquid chromatography coupled with diode array detection (HPLC-DAD), has been devised for the quantification of multiclass pesticides in aquatic samples. This methodology employs 1-Hexyl-3-methylimidazolium hexafluorophosphate ([C₁₀H₁₉N₂][PF₆]), 1-Octyl-3-methylimidazolium hexafluorophosphate ([C₁₂H₂₃N₂][PF₆]), and 1‑butyl‑3-methylimidazolium hexafluorophosphate ([C₈H₁₅N₂][PF₆]) as the extraction solvent and utilizes methanol as the disperser solvent. Critical parameters influencing the efficacy of the extraction, encompassing the type and volume of extraction and disperser solvents, sample pH, and vortex conditions, were meticulously optimized. Under optimal conditions, the methodology exhibited commendable linearity (0.9974 ≤ R<sup>2</sup> ≤ 0.9996), minimal limits of detection (0.1–1.3 µg/L) and quantification (0.3–3.9 µg/L), as well as satisfactory precision (relative standard deviation (RSD) ≤ 9.6 %). The methodology was adeptly applied to the analysis of tap water, groundwater, and river water samples, yielding recoveries spanning from 85 % to 105 %. The findings substantiate that IL-DLLME represents an auspicious technique for the extraction and quantification of multiclass pesticides in intricate aqueous matrices.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"8 ","pages":"Article 100231"},"PeriodicalIF":0.0,"publicationDate":"2025-06-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144272211","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}
引用次数: 0
Capsule phase microextraction methodology: Applications and future perspective 胶囊相微萃取方法:应用与展望
Journal of chromatography open Pub Date : 2025-05-01 DOI: 10.1016/j.jcoa.2025.100228
Shaikh Manirul Haque , Abuzar Kabir , Torki Zughaibi , Noorfatimah Yahaya , Bharti Jain , Rajeev Jain , Masoom Raza Siddiqui
{"title":"Capsule phase microextraction methodology: Applications and future perspective","authors":"Shaikh Manirul Haque ,&nbsp;Abuzar Kabir ,&nbsp;Torki Zughaibi ,&nbsp;Noorfatimah Yahaya ,&nbsp;Bharti Jain ,&nbsp;Rajeev Jain ,&nbsp;Masoom Raza Siddiqui","doi":"10.1016/j.jcoa.2025.100228","DOIUrl":"10.1016/j.jcoa.2025.100228","url":null,"abstract":"<div><div>Extraction plays a crucial role in the quantitative analysis of analytes across various matrices, particularly in biological and other complex samples, where accurate detection and determination would be challenging without effective extraction. Over time, new extraction techniques have been developed to meet evolving analytical needs. Nevertheless, sample preparation often still involves conventional steps such as analyte extraction, filtration, protein precipitation, centrifugation, elution with organic solvents, and solvent evaporation.</div><div>Among the latest advancements in this field is the Capsule Phase Microextraction (CPME) methodology, a green and sustainable technique. A key advantage of CPME is the reusability of microextraction capsules, which enhances cost-efficiency and environmental friendliness. The technique employs inorganic–organic hybrid sorbents and integrates multiple functions, such as filtration and diffusion, within a single device, thereby simplifying the extraction workflow.</div><div>This review highlights various aspects of the CPME methodology, including a schematic overview of the extraction process and the instrumentation used for post-extraction analysis. It also provides detailed information on the types of sorbents and eluting solvents utilized, along with the specific analytes effectively extracted using this technique.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100228"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144231529","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}
引用次数: 0
Improvement in protein separation by pH excursion modulated ion-exchange chromatography pH偏移调制离子交换色谱法对蛋白质分离的改进
Journal of chromatography open Pub Date : 2025-05-01 DOI: 10.1016/j.jcoa.2025.100229
Raja Ghosh
{"title":"Improvement in protein separation by pH excursion modulated ion-exchange chromatography","authors":"Raja Ghosh","doi":"10.1016/j.jcoa.2025.100229","DOIUrl":"10.1016/j.jcoa.2025.100229","url":null,"abstract":"<div><div>The transient change in pH during the elution step in ion exchange chromatography is commonly referred to as pH excursion. Acidic pH excursion is usually observed during salt-based elution in cation exchange chromatography. This could have a detrimental effect on protein stability as well as on protein separation. Acidic pH excursion could delay protein elution and thereby decrease resolution of sequentially eluted proteins. In a recent study, a method for suppressing or modulating pH excursion has been discussed. In the current study, the feasibility of using this approach for increasing resolution in protein separation is examined. Modulation of pH excursion during elution resulted in the rapid release of a weakly bound protein from cation exchange media while the release of a strongly bound protein remained largely unaffected. This differential effect was utilized to increase the resolution in binary protein separation. The resolution obtained in pH excursion modulated cation exchange chromatography was significantly greater than that obtained with unmodulated (or control) cation exchange chromatography, i.e., where acidic pH excursion was allowed to happen as usual. This approach for increasing resolution in protein separation could potentially be utilized in different analytical and preparative protein chromatography applications.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100229"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144205390","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}
引用次数: 0
Isolation of amyloidogenic aggregates of transthyretin by ceramic hydroxyapatite chromatography 陶瓷羟基磷灰石色谱法分离转甲状腺素淀粉样蛋白聚集体
Journal of chromatography open Pub Date : 2025-05-01 DOI: 10.1016/j.jcoa.2025.100223
Maria K. Tsoumpra , Shintaro Kobayashi , Eri Chatani
{"title":"Isolation of amyloidogenic aggregates of transthyretin by ceramic hydroxyapatite chromatography","authors":"Maria K. Tsoumpra ,&nbsp;Shintaro Kobayashi ,&nbsp;Eri Chatani","doi":"10.1016/j.jcoa.2025.100223","DOIUrl":"10.1016/j.jcoa.2025.100223","url":null,"abstract":"<div><div>Amyloidogenic proteins can lapse into unstable monomeric precursors which misfold and self-assemble into toxic oligomers and amyloid aggregates leading to intracellular deposition of insoluble amyloid fibrils, the hallmark of amyloidosis and major neurodegenerative diseases. The assembly pathway in amyloid diseases presents strong similarities regardless of the culprit protein and highly purified structures are required for its characterization. Herein, we have successfully separated tetrameric form from aggregated versions of the acidic amyloidogenic protein transthyretin (TTR), by a single step purification using ceramic hydroxyapatite (CHT) media. Native TTR elution from CHT media is phosphate-dependent, achieved at approximately 30 mM sodium phosphate. Adoption of a mild acetate environment favoured conversion of native TTR to a heterogeneous mixture with particles of 10–500 nm diameter and characteristics mimicking amyloid cascade components. We best explored the metal affinity and cation exchange dual CHT separation mechanism by generating a novel purification protocol that allowed for binding of TTR mixture at high salt presence, and distinct elution of tetramer and aggregate via application of a phosphate desalting gradient. We deduce that tetrameric version binds to the calcium site of CHT whereas amyloid aggregation uses both the calcium and phosphate binding sites of CHT, making it a suitable target for mixed-mode purification. The presence of granular aggregates was confirmed via transmission electron microscopy. Collectively, the data highlight the strength of hydroxyapatite as purification media in the rapidly expanding amyloidosis medical research field.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100223"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143921579","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}
引用次数: 0
Exploration of comprehensive two-dimensional liquid chromatography: Theoretical aspects and practical considerations - A tutorial 探索全面的二维液相色谱:理论方面和实际考虑-教程
Journal of chromatography open Pub Date : 2025-05-01 DOI: 10.1016/j.jcoa.2025.100222
Katia Arena , Francesco Cacciola , Roberto Laganà Vinci , Paola Dugo , Luigi Mondello
{"title":"Exploration of comprehensive two-dimensional liquid chromatography: Theoretical aspects and practical considerations - A tutorial","authors":"Katia Arena ,&nbsp;Francesco Cacciola ,&nbsp;Roberto Laganà Vinci ,&nbsp;Paola Dugo ,&nbsp;Luigi Mondello","doi":"10.1016/j.jcoa.2025.100222","DOIUrl":"10.1016/j.jcoa.2025.100222","url":null,"abstract":"<div><div>Comprehensive two-dimensional liquid chromatography (LC×LC) is a valuable tool for the analysis of very complex samples. LC×LC, which involves the coupling of two or more orthogonal separation systems, is a potential alternative to the conventional liquid-chromatography (1D-LC) approach. The profits of such a technique, compared to the 1D-LC approach, are the increased resolving power along with significant reduced ion enhancement or suppression phenomena in the MS source. This tutorial aims to provide detailed information on theoretical and practical aspects of the LC×LC approach with a particular focus on column combination, method optimization and separation performance. In addition, future perspectives and new trends are highlighted.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100222"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143946649","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}
引用次数: 0
New silicon phthalocyanine-containing polysiloxanes as stationary phases for high-temperature gas chromatography analysis 新型含酞菁硅聚硅氧烷作为固定相用于高温气相色谱分析
Journal of chromatography open Pub Date : 2025-05-01 DOI: 10.1016/j.jcoa.2025.100221
Mihaela-Liliana Ţînţaş , Valérie Peulon-Agasse , Marco Piparo , Pierre Giusti , Jean-Maurice Mallet , Pascal Cardinael
{"title":"New silicon phthalocyanine-containing polysiloxanes as stationary phases for high-temperature gas chromatography analysis","authors":"Mihaela-Liliana Ţînţaş ,&nbsp;Valérie Peulon-Agasse ,&nbsp;Marco Piparo ,&nbsp;Pierre Giusti ,&nbsp;Jean-Maurice Mallet ,&nbsp;Pascal Cardinael","doi":"10.1016/j.jcoa.2025.100221","DOIUrl":"10.1016/j.jcoa.2025.100221","url":null,"abstract":"<div><div>In this work a series of thermoresistant polysiloxanes containing silarylene units and macrocyclic silicon phthalocyanine (Pc) units (<strong>PS-1</strong> – <strong>PS-6</strong>) were synthesized. The Pc is linked to the polymer chain through a siloxane central group, which has two covalent bonds with two nitrogen atoms of the macrocycle and two covalent bonds with the polymer chain. The sol‒gel method led to the formation of polymeric chains with a random arrangement of monomers and OH-terminated chains. Thermogravimetric analyses revealed that the polymers are stable at high temperatures exhibiting, with a weight loss of 10 % between 384 and 442 °C during heating.</div><div>Coated as stationary phases for gas chromatography, polymers <strong>PS-1, PS-2</strong> and <strong>PS-5</strong> showed good film-forming ability. The columns prepared with <strong>PS-1</strong> and <strong>PS-5</strong> had 3300 and 3800 plates <em>m</em><sup>−1</sup>, respectively, as determined using pentadecane at 130 °C for fused silica capillary columns with an internal diameter of 250 µm, a film thickness of 0.25 µm and a length of 10 m. Polarity was estimated as moderate polarity (Rohrschneider–McReynolds constants were between 841 and 916) and stationary phases can achieve very good separation of Grob’s mixture, polycyclic aromatic hydrocarbons and essential oils. In addition, the columns provided excellent high temperature stability with very low bleeding (17.0 pA at 420 °C). Repeated injections of high boiling analytes revealed that <strong>PS-1</strong> is the most stable stationary phase at very high temperatures, as the smallest decrease of retention times (9.2 s) were observed after 50 successive injections (temperature program from 40 °C (hold 3 min) at 7 °C/min to 420 °C (hold 2 min). Moreover, it has been demonstrated that <strong>PS-1</strong> is more stable than commercial high-temperature columns such as ZB-XLB-HT and ZB-35HT (35 % phenyl/65 % dimethylpolysiloxane) from Phenomenex®.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100221"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143899746","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}
引用次数: 0
Use of tri-methylated-β-cyclodextrin and sub-2 μm silica particles for enantiomers separation by nano-liquid chromatography 利用三甲基化-β-环糊精和亚2 μm二氧化硅颗粒对映体进行纳米液相色谱分离
Journal of chromatography open Pub Date : 2025-05-01 DOI: 10.1016/j.jcoa.2025.100225
G. D’Orazio , S. Fanali
{"title":"Use of tri-methylated-β-cyclodextrin and sub-2 μm silica particles for enantiomers separation by nano-liquid chromatography","authors":"G. D’Orazio ,&nbsp;S. Fanali","doi":"10.1016/j.jcoa.2025.100225","DOIUrl":"10.1016/j.jcoa.2025.100225","url":null,"abstract":"<div><div>A short capillary column packed with RP18 sub-2 µm particles was investigated for enantioseparation of selected racemic acidic compounds such as nonsteroidal anti-inflammatory drugs (carprofen, cicloprofen, fenoprofen, flurbiprofen, ibuprofen, indoprofen, ketoprofen, naproxen, and suprofen) using a lab-made nano-liquid chromatography (nano-LC) system at conventional pressure conditions. The chiral separations were achieved by adding to the mobile phase heptakis (2,3,6-tri-O-methyl)-β-cyclodextrin (TM-β-CD) as the chiral additive. A comparative study with a 3 µm silica-based RP18 stationary phase highlights the crucial role of the stationary phase type. Despite similar or slightly higher enantioresolution factors, the most significant effects were the shorter analysis times (up to half) and higher theoretical plate numbers (estimated between 45,000 and 75,000 N/m) resulting from the reduced particle size of the stationary phase. This enabled a comprehensive organic solvent and aqueous content study, revealing valuable chromatographic insights. At a flow rate of approximately 400 nL/min, the most favourable mobile phase for enantiodiscrimination was achieved using 30 mM TM-β-CD in MeOH with a buffer pH 3.0. In line with the principles of Green Analytical Chemistry (GAC) and adhering to the White Analytical Chemistry principles, various tools were employed to assess the environmental impact of the method. These included the Analytical Eco-Scale, the Analytical GREEnness metric approach, and the Blue Applicability Grade Index that evaluated the miniaturized analytical methodology proposed aligned with the principles of Green Analytical Chemistry.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100225"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144196101","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}
引用次数: 0
Development and validation of a sensitive liquid chromatography-tandem mass spectrometry method for the analysis of Mancozeb residues in cauliflower: Risk assessment of real samples 菜花中代森锰锌残留的液相色谱-串联质谱分析方法的建立与验证:真实样品的风险评估
Journal of chromatography open Pub Date : 2025-05-01 DOI: 10.1016/j.jcoa.2025.100226
K. Tripathi , T. Harshangkumar , N. Narayanan , S. Gupta , S.B. Singh , T. Banerjee
{"title":"Development and validation of a sensitive liquid chromatography-tandem mass spectrometry method for the analysis of Mancozeb residues in cauliflower: Risk assessment of real samples","authors":"K. Tripathi ,&nbsp;T. Harshangkumar ,&nbsp;N. Narayanan ,&nbsp;S. Gupta ,&nbsp;S.B. Singh ,&nbsp;T. Banerjee","doi":"10.1016/j.jcoa.2025.100226","DOIUrl":"10.1016/j.jcoa.2025.100226","url":null,"abstract":"<div><div>The Dithiocarbamate (DTC) group represents one of the largest consumed fungicides. Presently the most extensively used UV–Visible spectrophotometric method for quantification of DTCs suffers from a lack of sensitivity for trace level detection of residue, poor stability, poor reproducibility, inability to determine LOD, LOQ and chances of matrix interference. In this study a sensitive residue analysis method has been developed and validated for the estimation of dithiocarbamate fungicide, Mancozeb, in cauliflower. Mancozeb was derivatized to a yellow coloured cupric dithiocarbamate complex, which was quantified with mass confirmation by LC–MS/MS. The LC-MS/MS method is considerably more sensitive (LOQ 0.01 µg g<sup>-1</sup>) than the UV–Visible (LOQ 0.1 µg g<sup>-1</sup>), specific (unique MRM transitions), accurate (recovery ∼93 %), precise (HorRat ∼0.3 at LOQ), rugged and associated with well acceptable uncertainty. 80 % of the real samples of cauliflower collected contain residues of DTCs above LOQ. Risk assessment of the real sample with the highest DTC contamination (0.18 µg g<sup>-1</sup>) was conducted. The Theoretical Maximum Residual Contribution (TMRC) of 0.027 mg of Mancozeb/person/day in the Katrain sample was found to be much less than the Maximum Permissible Intake (MPI) of 1.65 mg of mancozeb/person/day and it can be considered safe for human consumption.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100226"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144184341","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}
引用次数: 0
Determination of the composition and monosaccharide content of atractylodes polysaccharides using pre-column derivatization and a quantitative analysis of multicomponents by a single marker method 柱前衍生法测定苍术多糖的组成和单糖含量,单标记法测定多组分
Journal of chromatography open Pub Date : 2025-05-01 DOI: 10.1016/j.jcoa.2025.100224
Xiangyan Tu , Yueyue Wang , Jianwei Liu , Yingzhe Li , Yang Lu , Chunying Zhao , Zhongsi Li
{"title":"Determination of the composition and monosaccharide content of atractylodes polysaccharides using pre-column derivatization and a quantitative analysis of multicomponents by a single marker method","authors":"Xiangyan Tu ,&nbsp;Yueyue Wang ,&nbsp;Jianwei Liu ,&nbsp;Yingzhe Li ,&nbsp;Yang Lu ,&nbsp;Chunying Zhao ,&nbsp;Zhongsi Li","doi":"10.1016/j.jcoa.2025.100224","DOIUrl":"10.1016/j.jcoa.2025.100224","url":null,"abstract":"<div><div>Atractylodes chinensis (DC.) Koidz. (ACK), a prominent herb in traditional Chinese medicine, is widely used to treat conditions such as dampness obstruction in the middle Jiao, epigastric distension, diarrhea, and edema. The primary bioactive components of ACK include sesquiterpenes, alkynes, triterpenes, and polysaccharides. In this study, a high-performance liquid chromatography (HPLC) method with pre-column derivatization using 1-phenyl-3-methyl-5-pyrazolone (PMP) was developed. Additionally, a quantitative analysis of multicomponents by a single marker (QAMS) method was established to quantify polysaccharide components in ACK with high precision. Atractylodes chinensis polysaccharides (ACP) underwent acid hydrolysis with hydrochloric acid, yielding stable monosaccharide-PMP derivatives through pre-column derivatization. These derivatives were analyzed by HPLC, with anhydrous glucose as the internal standard. The relative correction factors for glucuronic acid, galactose, and arabinose were calculated using the QAMS method, yielding values of 1.08, 0.97, and 0.75, respectively. The monosaccharide contents determined by QAMS showed no significant difference from those obtained by the external standard method (ESM), with all relative standard deviations (RSD%) &lt;2 %. This method exhibited good linearity—linear ranges: glucuronic acid (0.0250–0.1250 mg/mL, r = 0.9996), anhydrous glucose (0.0094–0.0472 mg/mL, r = 0.9996), galactose (0.0100–0.0500 mg/mL, r = 0.9997), arabinose (0.0250–0.1250 mg/mL, r = 0.9987)—and the RSD% values for the stability of these four components within 48 hours were all &lt;3 %. In terms of reproducibility, multiple injections (<em>n</em> = 6) showed low relative standard deviations (RSD%): glucuronic acid (2.04 %), anhydrous glucose (0.32 %), galactose (0.53 %), arabinose (0.53 %). Regarding stability, within [specific time range], the RSD% values were: glucuronic acid (1.71 %), anhydrous glucose (2.49 %), galactose (2.11 %), arabinose (1.76 %). The accuracy was also satisfactory, with an RSD% of 3.45 %. These findings indicate that the established approach is robust, reliable, and applicable for determining monosaccharide content in hydrolyzed ACP. This methodology provides a promising tool for quality control and further pharmacological studies of ACP.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100224"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144069622","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}
引用次数: 0
Disposable in-tip cellulose paper device functionalized with clove essential oil for green and efficient extraction of abusable prescription drugs 用丁香精油功能化的一次性尖端纤维素纸装置,绿色高效地提取可滥用的处方药
Journal of chromatography open Pub Date : 2025-05-01 DOI: 10.1016/j.jcoa.2025.100227
Torki A. Zughaibi , Rajeev Jain
{"title":"Disposable in-tip cellulose paper device functionalized with clove essential oil for green and efficient extraction of abusable prescription drugs","authors":"Torki A. Zughaibi ,&nbsp;Rajeev Jain","doi":"10.1016/j.jcoa.2025.100227","DOIUrl":"10.1016/j.jcoa.2025.100227","url":null,"abstract":"<div><div>A novel, green, and cost-effective microextraction method based on a disposable-in-tip cellulose paper (DICP) device was developed for the determination of three commonly abused prescription drugs; dextromethorphan (DXM), tramadol (TRM), and clozapine (CLZ); in human urine samples. The DICP device was fabricated by dip-coating cellulose paper with 1 % clove essential oil (CEO), which imparts amphiphilic properties to the cellulose surface, enhancing its sorptive interaction with analytes of moderate polarity. The extraction was carried out using 50 manual aspiration–dispensing cycles, followed by 40 aspiration–dispensing cycles for desorption of target analytes with 500 µL of methanol. The proposed method is extremely cost-effective and high-throughput, enabling the preparation of 12 samples per hour, with 30 extraction strips obtained from a single cellulose disc. The mechanism of extraction relies on the synergistic interaction between cellulose hydroxyl groups and the eugenol-rich CEO layer, facilitating the adsorption of analytes through combined hydrophilic and hydrophobic interactions. The method demonstrated excellent analytical performance, with limit of quantifications (LOQs) between 0.06–0.09 µg mL<sup>-1</sup>, linearity (R² &gt; 0.994), intra-day and inter-day precision below 7 % and 13 %, respectively, and accuracy ranging from 86 to 110 %. Blind urine sample analysis confirmed the method’s reliability for real-world application. Furthermore, the protocol achieved a click analytical chemistry index (CACI) score of 85 and a ComplexMoGAPI score of 83, highlighting its outstanding greenness, simplicity, and field-deployability for forensic and toxicological applications.</div></div>","PeriodicalId":93576,"journal":{"name":"Journal of chromatography open","volume":"7 ","pages":"Article 100227"},"PeriodicalIF":0.0,"publicationDate":"2025-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144231620","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}
引用次数: 0
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