Journal of Chromatography A最新文献

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Fabrication of a green double-layered hybrid nanocomposite via electrospinning of polyethersulphone/natural deep eutectic solvent on bacterial cellulose for determination of multiclass pesticides in water samples 通过在细菌纤维素上电纺丝聚醚砜/天然深共晶溶剂制备绿色双层混合纳米复合材料,用于测定水样中的多类农药。
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-09-05 DOI: 10.1016/j.chroma.2024.465267
{"title":"Fabrication of a green double-layered hybrid nanocomposite via electrospinning of polyethersulphone/natural deep eutectic solvent on bacterial cellulose for determination of multiclass pesticides in water samples","authors":"","doi":"10.1016/j.chroma.2024.465267","DOIUrl":"10.1016/j.chroma.2024.465267","url":null,"abstract":"<div><p>A novel nanofibrous double-layered biosorbent was fabricated by electrospinning polyethersulfone (PES) doped with a natural deep eutectic solvent (DES), composed of choline chloride (ChCl) and caffeic acid (CFA) in a 3:1 molar ratio, onto a bacterial cellulose (BC) substrate. The pristine PES/DES@BC biosorbent was employed in a thin film-solid phase microextraction (TF-SPME) to extract 12 multiclass pesticides from water. Characterization techniques, including ATR-FTIR, FT-NMR, SEM, and nitrogen adsorption/desorption isotherms, confirmed the nanofibrous structure of the electrospun PES-DES and BC biopolymer. The method was validated for matrix effect, specificity, reproducibility, limits of quantification (0.03–0.10 µg/L), and enrichment factor (7–14). Matrix-match calibration linearity ranged from 0.03 to 500 μg/L, with determination coefficients (r²) between 0.9884 and 0.9994. Intra-day and inter-day relative standard deviations (RSDs) were 1.2–3.6 % and 7.0–9.3 %, respectively. The composition of the biosorbent and the fabrication reproducibility across different batches were also thoroughly examined. The accuracy was evaluated by measuring extraction recoveries in six environmental water samples, which ranged from 75 to 105 % (RSDs &lt; 9.0 %). Furthermore, the sustainability of the method was evaluated with the Analytical Eco-Scale and Analytical Greenness metrics. To our knowledge, this study represents the first synthesis and combination of [ChCl:[CFA] DES with PES to create a double-layered nanofiber biosorbent, as well as its application for extracting various pesticide groups from water samples.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-09-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142144737","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Accurate measurement of Soret coefficients in binary hydrocarbons mixtures based on composite methods 基于复合方法精确测量二元碳氢化合物混合物中的索雷特系数。
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-09-04 DOI: 10.1016/j.chroma.2024.465346
{"title":"Accurate measurement of Soret coefficients in binary hydrocarbons mixtures based on composite methods","authors":"","doi":"10.1016/j.chroma.2024.465346","DOIUrl":"10.1016/j.chroma.2024.465346","url":null,"abstract":"<div><p>The Soret effect is a significant factor in various scenarios, with thermodiffusion in binary systems serving as a common method for the study. Most research focuses rarely on the distribution characteristics of components in diffusion systems; and Soret coefficients in the porous media could not be obtained by typical methods based on the thermodiffusion column, which are particularly important in the field of oil and gas development. Moreover, experiments on ground conditions have struggled to determine the Soret coefficient accurately due to the convective effect caused by gravity differentiation. The thermodiffusion behavior of n-pentane (C5) and n-heptane (C7) binary mixtures in both bulk and porous media conditions have been investigated, aiming to provide corrected coefficients that mitigate the influence of gravity using theoretical derivation. A new method was proposed to calculate the Soret coefficients in this work by establishing a model based on gas chromatography technology. Dynamic variation of component concentration along the path was studied, and the corresponding Soret coefficients were calculated and analyzed in parallel. The results indicate that the concentration and temperature exhibit a logarithmic relationship with the distance from the heat source. The Soret coefficient values obtained from measurements in porous media are closer to the theoretically corrected values, which do not account for gravity effects. Additionally, as the permeability decreases, the counteracting effect of porous media on convection becomes more pronounced. Therefore, it presents a novel method for accurately measuring the Soret coefficient that ignores convection to some extent.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142144735","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Spherical cellulose/chitosan aerogel–supported MOF-199 for the magnetic solid-phase extraction of benzodiazepines from urine 球形纤维素/壳聚糖气凝胶支撑的 MOF-199,用于从尿液中磁性固相萃取苯并二氮杂卓类药物
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-09-04 DOI: 10.1016/j.chroma.2024.465347
{"title":"Spherical cellulose/chitosan aerogel–supported MOF-199 for the magnetic solid-phase extraction of benzodiazepines from urine","authors":"","doi":"10.1016/j.chroma.2024.465347","DOIUrl":"10.1016/j.chroma.2024.465347","url":null,"abstract":"<div><p>Metal–organic frameworks (MOFs) are promising materials for sample pretreatment. The performance improvement of powdered MOFs is hindered by their aggregation and difficult recovery. To overcome these issues, a biodegradable lightweight spherical aerogel was used as a support for the in situ growth of copper-based MOFs (MOF-199). Furthermore, Fe<sub>3</sub>O<sub>4</sub> nanoparticles were incorporated into the aerogel to achieve magnetic properties. Thus, hybrid aerogel spheres containing MOF-199 supported on magnetic oxidized cellulose nanofiber/carboxymethyl chitosan (MOF-199@mag-CNF/CMC) were fabricated. The effects of Fe<sub>3</sub>O<sub>4</sub> loading amount and organic-ligand concentration on the properties (spherical geometry and mechanical strength) of the hybrid aerogel spheres were studied. Their potential application in the extraction of benzodiazepines (BZPs) from urine samples prior to liquid chromatography–mass spectrometry was evaluated. The highly dispersed MOF-199 crystals on the spherical aerogel effectively overcame the inherent structural shrinkage of the bare aerogel spheres; thus, the MOF-199@mag-CNF/CMC aerogel spheres were robust and could withstand repeated use for at least eight consecutive extraction cycles. Further, MOF-199@mag-CNF/CMC exhibited improved BZP extraction efficiency, which was 2.5–11.6 times higher than that of bare Cu<sup>2+</sup>@mag-CNF/CMC aerogel spheres, primarily due to additional π–π interaction and H-bonding as well as improved specific surface area. Parameters influencing the extraction and desorption processes were also comprehensively investigated. Under optimal conditions, this method provided a wide linear range of 0.1–10 µg/L (<em>R</em><sup>2</sup> &gt; 0.995) and good precision (2.8–6.7% for intra-day; 1.9–7.8 % for inter-day). The limits of detection and quantification ranged from 0.02 to 0.11 µg/L and from 0.06 to 0.33 µg/L, respectively. The recoveries for the urine samples spiked with three concentrations of BZPs ranged from 73.9 % to 114.1 %. The proposed method is simple, sensitive and eco-friendly and can be used for the determination of BZPs from urine for clinical and forensic examinations.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142149305","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Hydrophilic interaction liquid chromatography: An efficient tool for assessing thorium interaction with phosphorylated biomimetic peptides 亲水相互作用液相色谱法:评估钍与磷酸化仿生肽相互作用的有效工具。
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-09-03 DOI: 10.1016/j.chroma.2024.465341
{"title":"Hydrophilic interaction liquid chromatography: An efficient tool for assessing thorium interaction with phosphorylated biomimetic peptides","authors":"","doi":"10.1016/j.chroma.2024.465341","DOIUrl":"10.1016/j.chroma.2024.465341","url":null,"abstract":"<div><p>In the field of nuclear toxicology, the knowledge of the interaction of actinides (An) with biomolecules is of prime concern in order to elucidate their toxicity mechanism and to further develop selective decorporating agents. In this work, we demonstrated the great potential of hydrophilic interaction liquid chromatography (HILIC) to separate polar thorium (Th) biomimetic peptide complexes, as a key starting point to tackle these challenges. Th<sup>4+</sup> was used as plutonium (Pu<sup>4+</sup>) analogue and pS16 and pS1368 as synthetic di- and tetra-phosphorylated peptides capable of mimicking the interaction sites of these An in osteopontin (OPN), a hyperphosphorylated protein. The objective was to determine the relative affinity of pS16 and pS1368 towards Th<sup>4+</sup>, and to evaluate the pS1368 selectivity when Th<sup>4+</sup> was in competition complexation reaction with UO<sub>2</sub><sup>2+</sup> at physiological pH. To meet these aims, HILIC was simultaneously coupled to electrospray ionization mass spectrometry (ESI-MS) and inductively coupled plasma mass spectrometry (ICP-MS), which allowed to identify online the molecular structure of the separated complexes and quantify them, in a single step. Dedicated HILIC conditions were firstly set up to separate the new dimeric Th<sub>2</sub>(peptide)<sub>2</sub> complexes with good separation resolution (peptide = pS16 or pS1368). By adding pS16 and pS1368 in different proportions relatively to Th<sup>4+</sup>, we found that lower or equal proportions of pS16 with respect to pS1368 were not sufficient to displace pS1368 from Th<sub>2</sub>pS1368<sub>2</sub> and pS16 proportion higher than pS1368 led to the formation of a predominant ternary complex Th<sub>2</sub>(pS16)(pS1368), demonstrating preferential Th<sup>4+</sup> binding to the tetra-phosphorylated peptide. Finally, online identification and quantification of the formed complexes when Th<sup>4+</sup> and UO<sub>2</sub><sup>2+</sup> were mixed in equimolar ratio relatively to pS1368 showed that in spite of pS1368 has been specifically designed to coordinate UO<sub>2</sub><sup>2+</sup>, pS1368 is also Th<sup>4+</sup>-selective and exhibits stronger affinity for this latter than for UO<sub>2</sub><sup>2+</sup>. Hence, the results gathered through this approach highlight the impact of Th<sup>4+</sup> coordination chemistry on its interaction with pS1368 and more widely to its affinity for biomolecules.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-09-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S0021967324007155/pdfft?md5=462815f6329b391ff17e470aec13f563&pid=1-s2.0-S0021967324007155-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142144739","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Efficient enrichment and characterization of triterpenoid saponins from Platycodon grandiflorus roots 高效富集和鉴定桔梗根中的三萜类皂苷
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-09-02 DOI: 10.1016/j.chroma.2024.465332
{"title":"Efficient enrichment and characterization of triterpenoid saponins from Platycodon grandiflorus roots","authors":"","doi":"10.1016/j.chroma.2024.465332","DOIUrl":"10.1016/j.chroma.2024.465332","url":null,"abstract":"<div><p><em>Platycodon grandiflorum</em> roots (PGR), a widely recognized edible herbal medicine, are extensively used in traditional Chinese medicine for respiratory ailments. PGR are rich in bioactive compounds, particularly triterpenoid saponins, which possess significant pharmaceutical properties, including anti-inflammatory, antifungal, and antioxidant activities. Despite their recognized bioactivity, the purification and enrichment processes of triterpenoid saponins remain underexplored. This study aimed to optimize the extraction and purification of triterpenoid saponins from PGR to enhance resource utilization and minimize waste. Our method involved n-butanol extraction and macroporous adsorption resin, yielding four extracts with varying saponins contents. Qualitative analysis using LC-MS identified 8 triterpenoid saponins across the extracts. Further fragmentation analysis delineated characteristic ion patterns and cleavage pathways for these compounds. Quantitative analysis demonstrated that the separation and purification process effectively increased the triterpenoid saponins content, with the highest levels obtained through 30 % ethanol elution. Notably, the absence of Platycodin D in the 30 % ethanol eluate highlighted potential variations due to the origin, processing, and purification methods. These findings provide theoretical support for the development and utilization of triterpenoid saponins in PGR.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-09-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142144736","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Two-Dimensional Liquid Chromatography Purified GC/C/IRMS Doping Control Method: Analysis of Endogenous and Exogenous Sources in Urine Samples from Asian Subjects Administered a Low Dose of AICAR 二维液相色谱净化 GC/C/IRMS 兴奋剂控制方法:对服用低剂量 AICAR 的亚洲受试者尿样中的内源性和外源性来源进行分析
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-31 DOI: 10.1016/j.chroma.2024.465312
{"title":"Two-Dimensional Liquid Chromatography Purified GC/C/IRMS Doping Control Method: Analysis of Endogenous and Exogenous Sources in Urine Samples from Asian Subjects Administered a Low Dose of AICAR","authors":"","doi":"10.1016/j.chroma.2024.465312","DOIUrl":"10.1016/j.chroma.2024.465312","url":null,"abstract":"<div><p>AICAR (5-amino-4-imidazolecarboxyamide ribonucleoside), as a metabolic modulator, is classified in the S4 category by the World Anti-Doping Agency (WADA). Carbon Isotope Ratio Mass Spectrometry (CIR) is the mainstream method for distinguishing the endogenous and exogenous sources of AICAR in urine due to the significant individual difference in the concentration. The purpose of this study is to establish a gas chromatography combustion Isotope Ratio Mass Spectrometry (GC/C/IRMS) method for AICAR based on efficient two-dimensional liquid chromatography (2D-HPLC) separation.</p></div><div><h3>Method</h3><p>In this study, an automated 2D-HPLC separation technique was used to separate and purify AICAR and endogenous reference substances in urine samples. Then, AICAR was derivatized with 3-TMS as the main derivative product, while the endogenous reference compounds remained in their original form. Subsequently, the developed GC/C/IRMS method was utilized for the detection of the target and reference substances. Followed, we evaluated the applicability of this method using urine samples from two Asian males administered a low dose of AICAR (3 grams).</p></div><div><h3>Results</h3><p>The advantages of this study include: 1) reduced sample pretreatment time: the established 2D-HPLC separation method can separate the target and endogenous reference substances in one step; 2) low interference: the isotope chromatograms have low background interference, and the separation of endogenous reference substances is purer; 3) more accurate result calculations: this method only requires derivatization and result correction for AICAR, with the endogenous reference substances measured in their original form, reducing biases from corrections of multiple substances. The detection method performed well, with a concentriton limit of 2500 ng/mL, meeting the needs of routine detection concentrations. The CIR results from volunteer samples indicated that samples collected within 16 hours post-administration exceeded the threshold set in the literature.</p></div><div><h3>Conclusion</h3><p>This study successfully established a 2D-HPLC-GC/IRMS method that integrates CIR as the most stable indicator for distinguishing the internal and external sources of AICAR. After administering a low dose of AICAR to the Asian population, exogenous drug characteristics were manifested within 16 hours. This observation, when compared to the 40-hour detection window cited in the literature, suggests that the length of the detection window is positively correlated with the dosage of the test drug.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142128590","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Harnessing an elastic flow instability to improve the kinetic performance of chromatographic columns 利用弹性流动不稳定性改善色谱柱的动力学性能
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-31 DOI: 10.1016/j.chroma.2024.465326
{"title":"Harnessing an elastic flow instability to improve the kinetic performance of chromatographic columns","authors":"","doi":"10.1016/j.chroma.2024.465326","DOIUrl":"10.1016/j.chroma.2024.465326","url":null,"abstract":"<div><p>Despite decades of research and development, the optimal efficiency of slurry-packed HPLC columns is still hindered by inherent long-range flow heterogeneity from the wall to the central bulk region of these columns. Here, we show an example of how this issue can be addressed through the straightforward addition of a semidilute amount (500 ppm) of a large, flexible, synthetic polymer (18 MDa partially hydrolyzed polyacrylamide, HPAM) to the mobile phase (1% NaCl aqueous solution, hereafter referred to as “brine”) during operation of a 4.6 mm <span><math><mo>×</mo></math></span> 300 mm column packed with <span><math><mrow><mn>10</mn><mspace></mspace><mi>μ</mi><mi>m</mi></mrow></math></span> BEH<span><math><msup><mrow></mrow><mrow><mi>T</mi><mi>M</mi></mrow></msup></math></span> 125 Å particles. Addition of the polymer imparts elasticity to the mobile phase, causing the flow in the interparticle pore space to become unstable above a threshold flow rate. We verify the development of this elastic flow instability using pressure drop measurements of the friction factor versus Reynolds number. In prior work, we showed that this flow instability is characterized by large spatiotemporal fluctuations in the pore-scale flow velocities that may promote analyte dispersion across the column. Axial dispersion measurements of the quasi non-retained tracer thiourea confirm this possibility: they reveal that operating above the onset of the instability improves column efficiency by greater than 100%. These experiments thereby suggest that elastic flow instabilities can be harnessed to mitigate the negative impact of trans-column flow heterogeneities on the efficiency of slurry-packed HPLC columns. While this approach has its own inherent limitations and constraints, our results lay the groundwork for future targeted development of polymers that can impart elasticity when dissolved in commonly used liquid chromatography mobile phases, and can thereby generate elastic flow instabilities to help improve the resolution of HPLC columns.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142135937","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Preparation of ionic gel-modified stationary phase for RPLC/HILIC/IC separation and its application in per aqueous liquid chromatography 用于 RPLC/HILIC/IC 分离的离子凝胶改性固定相的制备及其在水相液相色谱中的应用。
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-31 DOI: 10.1016/j.chroma.2024.465313
{"title":"Preparation of ionic gel-modified stationary phase for RPLC/HILIC/IC separation and its application in per aqueous liquid chromatography","authors":"","doi":"10.1016/j.chroma.2024.465313","DOIUrl":"10.1016/j.chroma.2024.465313","url":null,"abstract":"<div><p>In this study, we synthesized and employed an ionic gel-functionalized silica stationary phase for high-performance liquid chromatography. The successful fabrication of the stationary phase was confirmed through attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR), X-ray photoelectron spectroscopy (XPS), zeta-potential measurements, and elemental analysis (EA). Comparative performance evaluation against a commercial column demonstrated the prepared column's effectiveness in the mixed mode of reversed-phase liquid chromatography (RPLC), hydrophilic interaction liquid chromatography (HILIC), and ion chromatography (IC). Moreover, the stationary phase exhibited exceptional retention repeatability in per aqueous liquid chromatography, showcasing its potential as an environmentally friendly analytical method. Mechanistic investigations unveiled multiple solute-stationary phase interactions, including π-π interactions, hydrogen bonding, and ion exchange. Finally, we applied the developed stationary phase for the precise detection of preservatives in carbonated beverages and jelly, achieving high levels of accuracy and recovery rates.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142144751","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
HPTLC-guided flash chromatographic isolation and spectroscopic identification of bioactive compounds from olive flowers HPTLC 引导的闪速色谱分离和光谱鉴定橄榄花中的生物活性化合物
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-31 DOI: 10.1016/j.chroma.2024.465310
{"title":"HPTLC-guided flash chromatographic isolation and spectroscopic identification of bioactive compounds from olive flowers","authors":"","doi":"10.1016/j.chroma.2024.465310","DOIUrl":"10.1016/j.chroma.2024.465310","url":null,"abstract":"<div><p>The goal of preparative chromatography is to isolate suitable amounts of compound(s) at the required purity in the most cost-effective way. This study analyses the power of High-performance thin-layer chromatography (HPTLC) guided preparative flash chromatography to separate and isolate bioactive compounds from an olive flower extract for their further characterisation via spectroscopy. The structure and purity of isolated bioactive compounds were assessed using Fourier-transform infrared (FTIR) and nuclear magnetic resonance (NMR) spectroscopy. Flash chromatography of the olive flower extract successfully isolated pure oleanolic and maslinic acids. Moreover, the flash chromatography of the extract allowed isolation and phytochemical analysis of the most lipophilic fraction of the extract, which was found to contain <em>n</em>-eicosane and <em>n</em>-(<em>Z</em>)-eicos-5-ene, that has not been isolated previously with preparative TLC.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S0021967324006848/pdfft?md5=f238c6d2d346532502ea512c02030b18&pid=1-s2.0-S0021967324006848-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142128591","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A multi-technique analytical approach to support (eco)toxicological investigation of zinc oxide nanoparticles 支持纳米氧化锌(生态)毒理学研究的多技术分析方法。
IF 3.8 2区 化学
Journal of Chromatography A Pub Date : 2024-08-31 DOI: 10.1016/j.chroma.2024.465331
{"title":"A multi-technique analytical approach to support (eco)toxicological investigation of zinc oxide nanoparticles","authors":"","doi":"10.1016/j.chroma.2024.465331","DOIUrl":"10.1016/j.chroma.2024.465331","url":null,"abstract":"<div><p>Understanding the mechanism of toxicity of nanoparticles and their behavior in biological environments is crucial for designing materials with reduced side effects and improved performance. Among the factors influencing nanoparticle behavior in biological environments, the release and bioavailability of potentially toxic metal ions can alter equilibria and cause adverse effects. In this study, we applied two on-line Field-Flow Fractionation (FFF) strategies and compared the results with off-line benchmarking centrifugal ultrafiltration to assess a key descriptor, namely the solubility of zinc oxide (ZnO) nanoparticles. We found that, at the highest nanoparticle concentrations, the nanoparticle-ion ratio quickly reaches equilibrium, and the stability is not significantly affected by the separation technique. However, at lower concentrations, dynamic, non-equilibrium behavior occurs, and the results depend on the method used to separate the solid from the ionic fraction, where FFF yielded a more representative dissolution pattern. To support the (eco)toxicological profiling of the investigated nanoparticles, we generated experimental data on colloidal stability over typical (eco)toxicological assay durations. The Zeta Potential vs pH curves revealed two distinct scenarios typical of surfaces that have undergone significant modification, most likely due to pH-dependent dissolution and re-precipitation of surface groups. Finally, to enhance hazard assessment screening, we investigated ion-dependent toxicity and the effects of exposure to fresh water. Using an in vitro human skin model, we evaluated the cytotoxicity of fresh and aged ZnO nanoparticles (exposed for 72 h in M7), revealing time-dependent, dose-dependent, and nanoparticle-dependent cytotoxicity, with lower toxicity observed in the case of aged samples.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142144734","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","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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