Journal of Chromatography A最新文献

{"title":"Utilization of AF4 for characterizing complex nanomaterial drug products: Reexamining sample recovery and its impact on particle size distribution as a quality attribute","authors":"Christine L. Plavchak ,&nbsp;Joanne Liu ,&nbsp;Yan Wang ,&nbsp;Xiaoming Xu ,&nbsp;Patrick J. Faustino ,&nbsp;Haiou Qu ,&nbsp;William C. Smith","doi":"10.1016/j.chroma.2025.465703","DOIUrl":"10.1016/j.chroma.2025.465703","url":null,"abstract":"<div><div>Asymmetrical flow field-flow fractionation (AF4) with multi-detection has continued to gain wider acceptance for characterizing complex drug products. An important quality attribute for these products is the measurement of the particle size distribution (PSD). Current limitations of established procedures (e.g., dynamic light scattering) for accurately determining PSD can be overcome by AF4. However, while gaining acceptance this technique has not been fully adopted within the pharmaceutical industry. A technical understanding of fundamental operational factors is necessary for the successful application of utilizing any emerging technology. For example, recovery (<em>R% = A_S/A_D*100_,</em> where <em>A_S</em> and <em>A_D</em> are the peak areas from the concentration detector with and without the crossflow field, respectively) is one factor that is used to assess the robustness during AF4 method development, but currently little is known about the interplay between analyte recovery and PSD. This work highlights factors that impact calculated AF4 recovery, and how differences in analyte and absolute recovery ultimately influence the PSD of nanoparticle size standards and complex drug product formulations such as emulsions and liposomes. Factors like ionic strength, buffer composition, and analyte chemistries, which are the most common factors associated with changes to <em>R%</em> in AF4, contributed to changes in <em>A_S</em>. While <em>A_D</em> is not typically examined in detail, the selection of the concentration detector (UV or dRI) along with their instrumental parameters (e.g., wavelength, attenuation value, linear range) and sample preparation was shown to under- or over-estimate <em>A_D</em> thus changing <em>R%</em>. Examining both components of <em>R%</em> and their contributions to analyte and absolute recovery show that decreases in analyte recovery may not be exclusively due to sample loss but could be influenced by changes in analyte-membrane interactions or analyte instability. Because of this, four relationships between recovery and PSD were defined. While <em>R%</em> is used as a tool for assessing AF4 methodology, the factors investigated through this work warrant further considerations when establishing an appropriate <em>R%</em> threshold.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465703"},"PeriodicalIF":3.8,"publicationDate":"2025-01-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143057664","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}

{"title":"Defect-rich Co/N-doped hierarchically porous carbons for rapid and highly efficient adsorption of organophosphorus pesticides from environmental water","authors":"Yaqing Zhao ,&nbsp;Yaming Sun ,&nbsp;Chenchen Song ,&nbsp;Hailiang Zhao ,&nbsp;Shiqi Chai ,&nbsp;Xuemeng Xu ,&nbsp;Lijun He","doi":"10.1016/j.chroma.2025.465700","DOIUrl":"10.1016/j.chroma.2025.465700","url":null,"abstract":"<div><div>Organophosphorus pesticides (OPPs) severely pollute various environmental water due to their excessive use, and it is extremely urgent to develop novel adsorbents with high adsorption capacities, rapid removal rate and easily recovery for the removal of OPPs. In this study, defect-rich Co/N-doped hierarchically porous carbons (Co/N-DHPCs) were constructed by pyrolyzing acid-etched ZIF-67 precursor. The developed Co/N-DHPCs possessed rich defects, well-developed hierarchical porous structure, high specific surface area and excellent magnetic property, and exhibited large adsorption capacities of 103.81∼126.10 mg g^-1 and high removal efficiencies of 94.06 %∼100.00 % for fenitrothion, fenthion and phosalone within 15 min. The exceptional adsorption performance of Co/N-DHPCs could be attributed to the pore-filling effect, hydrophobic and π-π interactions, as well as the new active sites formed by rich defects and N heteroatoms doping. In addition, the magnetic property of Co/N-DHPCs enabled rapid and straightforward separation from aqueous solution. The Co/N-DHPCs also showed good reusability with removal efficiencies of 85.24 % after five consecutive recycles. Furthermore, the developed Co/N-DHPCs demonstrated remarkable removal efficiencies of OPPs in seven environmental water samples, particularly in high-salt seawater. This work provides a kind of reliable adsorbents for removing pollutants in environmental water.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465700"},"PeriodicalIF":3.8,"publicationDate":"2025-01-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143035684","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}

{"title":"Simulation of the performance of pillar array columns using the pore-throat ratio as efficiency descriptor","authors":"Qihao Jiang ,&nbsp;Simone Dimartino","doi":"10.1016/j.chroma.2025.465704","DOIUrl":"10.1016/j.chroma.2025.465704","url":null,"abstract":"<div><div>Traditional packed beds in chromatography suffer from increased band broadening due to the random nature of packing, leading non-ideal fluid flow and channeling. To address these challenges, pillar array columns have been developed, offering improved performance over random packing thanks to their homogenous fluid profiles. The study aims to i) evaluate fluid dynamics and chromatographic performance across different PAC morphologies, ii) establish the influence of column morphology on performance, and iii) assess the correlation between chromatographic performance and hydrodynamic parameters. Approximately 200 PAC morphologies with different pillar shapes, pillar sizes, rotations and radial stretching were simulated using the finite element method (FEM). The pore-throat ratio was introduced as a predictor for separation efficiency, showing a strong positive correlation between this ratio and the minimum reduced plate height <span><math><msub><mi>h</mi><mrow><mi>m</mi><mi>i</mi><mi>n</mi></mrow></msub></math></span>. It is suggested that a more homogenous fluid profile, indicated by a pore-throat ratio approaching 1, is associated with higher column efficiency and permeability, allowing for larger optimal velocities and reduced separation time. For PACs, the <span><math><msub><mi>h</mi><mrow><mi>m</mi><mi>i</mi><mi>n</mi></mrow></msub></math></span> is close to 0.25 as the pore throat ratio approaches 1. The simplicity of calculating the pore-throat ratio from the column structure without the need for chromatographic experiments or modeling makes it a practical tool for predicting column performance.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465704"},"PeriodicalIF":3.8,"publicationDate":"2025-01-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143035709","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}

{"title":"Automatic monitoring and on-line chiral separation of chiral drug synthesis","authors":"Zhongmei Chi,&nbsp;Shiqi Chu,&nbsp;Jiali Gu,&nbsp;Guocheng Liu","doi":"10.1016/j.chroma.2025.465699","DOIUrl":"10.1016/j.chroma.2025.465699","url":null,"abstract":"<div><div>Chiral synthesis of single chiral drugs offers high efficiency, controllable costs, and excellent enantioselectivity, making it crucial in the pharmaceutical industry. A significant number of studies on chiral drug synthesis primarily focuses on the design and synthesis of innovative chiral catalysts and ligands with extremely high selectivity, as well as the development of new methods and strategies. Nonetheless, the on-line monitoring of chiral drug synthesis and its underlying mechanisms remain obscure. The principal challenge lies in the diverse synthesis pathways and intricate mechanisms of chiral drugs, with numerous intermediates and by-products. To tackle this issue, employing the chiral drug omeprazole as a breakthrough, we design and establish a reliable and stable analytical method to monitor the synthesis process. By integrating electrokinetic chromatography technology with automatic sequence injection, the chiral synthesis of omeprazole can be comprehensively tracked and monitored throughout its entire process. During the chiral drug synthesis process, all compounds, containing all reagents and products (omeprazole sulfide, R-omeprazole, S-omeprazole, iodobenzene and iodobenzene diacetate) are efficiently separated and simultaneously detected through a single run. The method shows a high resolution greater than 1.2, a wide linear range with a detection limit as low as 0.008 μM, as well as exceptional repeatability in sequence analysis. Therefore, the proposed method has demonstrated significant value in the analysis of chiral drug synthesis and holds potential for extensive application in the industrial production of chiral compound synthesis.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465699"},"PeriodicalIF":3.8,"publicationDate":"2025-01-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143035642","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}

{"title":"Enhanced adsorption capacity and specificity for recognition of low-density lipoprotein (LDL) with resorcinol-formaldehyde nanospheres and aptamer decorated graphene oxide nanocomposites","authors":"Jianfang Cao ,&nbsp;Peng Hu ,&nbsp;Pengfei Du ,&nbsp;Haili Wang ,&nbsp;Yanli Ma ,&nbsp;Weiting Wang","doi":"10.1016/j.chroma.2025.465697","DOIUrl":"10.1016/j.chroma.2025.465697","url":null,"abstract":"<div><div>Hypercholesterolemia is one of the major factors in the formation of atherosclerosis, and abnormally elevated low-density lipoprotein (LDL) levels are an essential indicator of the development of hypercholesterolemia. Selective reduction of LDL levels has attracted widespread attention as an important strategy for treating of hypercholesterolemia in the clinic. Here, based on the advantageous swelling properties of resorcinol-formaldehyde (RF) nanospheres, nanosorbents (GO/RF/Apt) with high adsorption capacity and high selectivity are prepared by a two-step amidation reaction for LDL adsorption studies. The optimal sorption capacity of GO/RF/Apt nanocomposites for LDL upto 3528.6 μg mg^-1 at the optimal experimental conditions. The utilization of the complementary single-stranded DNA for LDL-aptamer facilitates efficient LDL elution and shows superior elution efficiency. In addition, GO/RF/Apt nanocomposites as adsorbents exhibit promising adsorption behaviors toward LDL in the goat serum sample, demonstrating that GO/RF/Apt possesses the ability to selectively separate LDL from complex sample matrices. The successful application of GO/RF/Apt nanomaterials provides an innovative idea to the reduction of LDL levels in the clinic.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465697"},"PeriodicalIF":3.8,"publicationDate":"2025-01-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143078287","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}

{"title":"Strategy to mitigate aggregation during Protein A chromatography and low pH virus inactivation for a nivolumab biosimilar candidate","authors":"Elizabeth Pargas-Ferrer,&nbsp;Sum Lai Lozada Chang,&nbsp;Katia García,&nbsp;Ernesto Azaharez,&nbsp;Julio Palacio,&nbsp;Midalys Cabrera Mena,&nbsp;Tammy Boggiano-Ayo","doi":"10.1016/j.chroma.2025.465698","DOIUrl":"10.1016/j.chroma.2025.465698","url":null,"abstract":"<div><div>Protein A chromatography represents the most prevalent methodology for the capture of monoclonal antibodies. The use of a low pH elution buffer from Protein A has been observed to contribute to product aggregation, particularly in the case of IgG4 antibodies, such as nivolumab. This paper presents a well-defined strategy for addressing this issue. Initial experiments were conducted at scale-down Protein A affinity chromatography to evaluate the use of glycine-HCL and sodium citrate as elution buffers at pH values of 3.25, 3.5, and 3.75. Subsequently, a scale-down screening was conducted to assess the efficacy of various additives in Protein A elution. These included 10 % (w/v) mannitol, 50 mM histidine, 50 mM sucrose, 10 % (v/v) sorbitol, 50 mM arginine, 50 mM trehalose, 0.02 % (v/v) polysorbate 80, 1.5 M urea, and 1 M MgCl₂. The three most stabilizing additives were evaluated at the laboratory scale, and the one that demonstrated the greatest ability to maintain the minimum high molecular weight aggregate over time was selected. Lastly, the selected additive was subjected to testing at elevated IgG concentrations during purification. Nivolumab exhibits a markedly pH-dependent propensity for aggregation, and the relative efficacy of glycine-HCL and sodium citrate in mitigating anti-PD1 aggregation within the pH range of 3.25 to 3.75 is subject to variation. The use of buffer 100 mM sodium citrate, pH 3.5 was found to be beneficial. All additives evaluated contribute to reducing nivolumab aggregation, albeit in different ways and to varying degrees of effectiveness. Elution buffer with mannitol, polysorbate 80, or MgCl₂ resulted in a monomer control ratio of approximately twice that observed in the absence of additives. However, the stabilizing role of mannitol was confirmed to be particularly significant, as the ratio of aggregation formed at a low pH was reduced to ≤ 2 % from 15 % in all evaluated scales and at different protein concentrations, while maintaining high biological activity.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465698"},"PeriodicalIF":3.8,"publicationDate":"2025-01-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997681","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}

{"title":"Green synthesis of water-compatible layer-by-layer assembled sandwich bread-like molecularly imprinted polymers for selective recognition of baicalin from Scutellariae Radix","authors":"Yanhui Zhang ,&nbsp;Hongbo Li ,&nbsp;Xiaoqin Hai ,&nbsp;Qingxin Lu ,&nbsp;Jiaxiao Niu ,&nbsp;Ruiyu Fu ,&nbsp;Xiaoli Guo ,&nbsp;Xin Di","doi":"10.1016/j.chroma.2025.465673","DOIUrl":"10.1016/j.chroma.2025.465673","url":null,"abstract":"<div><div>Molecularly imprinted polymers (MIPs) are typically synthesized in organic solvents, leading to poor compatibility with water, weak affinity and selectivity for target molecules in aqueous media. To address these challenges, a green and sustainable synthesis of sandwich bread-like ATP@MIP was conducted using polyethylenimide (PEI) and deep eutectic solvent (DES) as hydrophilic bi-functional monomers via layer-by-layer self-assembly on the attapulgite (ATP) carrier. The new ATP@MIP can provide a higher density of imprinting sites with more orderly and uniform distribution due to inhibiting the competitive polymerization between PEI and DES, thereby significantly enhancing recognition ability. Moreover, the ATP@MIP was synthesized in water, aligning with green chemistry principles and establishing a sustainable preparation method for MIP materials. Equipped with the remarkable merits of good water compatibility, excellent selectivity (IF=3.6), high adsorption capacity (77.6 mg g⁻¹) and desirable repeatability (8 times), the as-prepared materials were used as a solid phase extraction adsorbent for efficient separation and enrichment of baicalin from <em>Scutellariae Radix</em>. More importantly, the recognizing performance of ATP@MIP for baicalin increased 1.40–1.69 times than other MIP materials, and its excellent specificity was demonstrated in comparison with several common commercial adsorbents (C18, HLB, MCX and SAX). Therefore, this work introduces a feasible and green strategy to synthesize water-compatible MIP materials for highly selective enrichment and separation of active components from natural products.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465673"},"PeriodicalIF":3.8,"publicationDate":"2025-01-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142997653","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}

{"title":"Analysis of partly bio-derived nonionic polyethylene glycol-based rheology modifiers by comprehensive two-dimensional liquid chromatography","authors":"Meng Jing ,&nbsp;Wenshiue Young ,&nbsp;Kathleen Michels ,&nbsp;Yujing Tan ,&nbsp;David Meunier ,&nbsp;Fanwen Zeng ,&nbsp;Shiling Zhang","doi":"10.1016/j.chroma.2025.465694","DOIUrl":"10.1016/j.chroma.2025.465694","url":null,"abstract":"<div><div>Rheology modifiers (RMs) are polymeric molecules providing rheological control of formulations, which are important in product application, shelf-life, and aesthetic perception. Bio-derived polyethylene glycol (PEG)-based RMs thicken formulations through nonionic-associative thickening where at least two hydrophobic end groups from a RM molecule interact with other hydrophobic groups of other RM molecules or ingredients in the formulation to form an associative network. We report a comprehensive two-dimensional liquid chromatography (2D-LC) separation of partly bio-derived PEG-based RMs in size exclusion chromatography (SEC) × reversed-phase liquid chromatography (RPLC) mode for the separation of RM components based on both molecular weight distribution and end group hydrophobe distribution. Matrix-assisted laser desorption ionization mass spectrometry (MALDI-MS) is first performed to gain understanding of the molecular weight, number of distributions, and approximate sample complexity, which helps with the SEC column selection. A thorough solubility screening is then conducted to identify the compatible SEC mobile phases and the gradient range for the RPLC column. Then, both SEC and RPLC methods are developed for the successful comprehensive SEC × RPLC separation of polymers with 0, 1, 2, 3, and 4 terminal hydrophobes. Finally, high resolution mass spectrometry mass profiler is used to further explain the minor secondary interaction mechanism of the SEC separation and confirm the MALDI results.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465694"},"PeriodicalIF":3.8,"publicationDate":"2025-01-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143021692","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}

{"title":"Deep Eutectic Solvents based green approach for bioactive molecules recovery from Spirulina","authors":"Susanna Della Posta,&nbsp;Erica Cutè,&nbsp;Laura De Gara,&nbsp;Chiara Fanali","doi":"10.1016/j.chroma.2025.465695","DOIUrl":"10.1016/j.chroma.2025.465695","url":null,"abstract":"<div><div>Spirulina is a unicellular microalga, characterized by blue/green color, that has received significant attention for its interesting nutritional composition. Phenolic compounds and phycocyanin (PC) are responsible for the many biological activities of Spirulina. Spirulina phenolic compounds are usually extracted using organic solvents, while PC is extracted with water or phosphate buffer solution, obtaining an extract characterized by low stability and low purity. Deep Eutectic Solvents (DESs) are green solvents, widely applied for bioactive molecules extraction, composed by two or more molecules which act as hydrogen bond acceptor or hydrogen bond donor to create an eutectic mixture. A Natural Deep Eutectic Solvent (NADES), is a DES composed only by natural compounds. This work aimed to optimize a green extraction procedure based on NADES to obtain an extract rich in phenolic compounds and PC from Spirulina. The application of NADESs as extraction solvents is an important strategy for recovering phenolic compounds and to increase and stabilize the protein PC. The optimized extraction procedure involved to use a betaine-glucose NADES under the following conditions: matrix-to-solvent ratio of 1:20 (w/w), temperature of 50 °C and one hour as extraction time. The developed extraction procedure guaranteed to recover a phenolic compounds and PC quantity of 11.77 ± 1.23 mg GAE (gallic acid equivalents) and 27.56 ± 2.46 g per g of Spirulina powder respectively. PC in the NADES extract degraded more slowly than in an aqueous extract. The extract phenolic compounds profile was determined through high performance liquid chromatography coupled with mass spectrometry analysis.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465695"},"PeriodicalIF":3.8,"publicationDate":"2025-01-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143021695","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}

{"title":"The application of design of experiments and artificial neural networks in the evaluation of the impact of acidic conditions on cloud point extraction","authors":"Bartosz Sznek,&nbsp;Andrzej Czyrski","doi":"10.1016/j.chroma.2025.465686","DOIUrl":"10.1016/j.chroma.2025.465686","url":null,"abstract":"<div><div>This study aimed to analyze the impact of acidic conditions on the recovery of ciprofloxacin and levofloxacin for cloud point extraction with the Design of Experiments and Artificial Neural Networks. The design included 27 experiments featuring three repetitions of the central point for both drugs. The tested parameters included Triton X-114 concentration, HCl concentration, NaCl concentration, and incubation temperature, which were coded at five levels. After extraction, samples were analyzed using HPLC, and statistical analysis was performed using Statistica software. Polynomial equations were developed to predict recovery values based on the experimental conditions. Results indicated that Triton X-114 concentration had the most significant impact on recovery for ciprofloxacin and levofloxacin, while HCl concentration also played an important role. The highest recovery for ciprofloxacin was observed for the following conditions: 8.5 % TX-114, 0.1 M HCl, temperature of incubation 45 °C, and no addition of NaCl. The highest recovery for levofloxacin was observed under the following conditions: 9 % TX-114, 1.5 M HCl, temperature of incubation 60 °C, and no addition of NaCl. The observed recoveries were 43 % and 53 % for levofloxacin and ciprofloxacin, respectively. They were in accordance with the predicted values calculated with DoE and with ANN approach, These findings validate the use of the Central Composite Design and Artificial Neural Networks for analyzing how acidic conditions affect the recovery of both drugs, allowing for detailed analysis and optimization of the influencing factors.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1743 ","pages":"Article 465686"},"PeriodicalIF":3.8,"publicationDate":"2025-01-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143027480","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}