Chromatographia最新文献

{"title":"Retraction Note: Stability Indicating and Green Solvent-Assisted Chromatographic Analysis of an Antiviral Drug","authors":"K. Archana, M. Sumithra","doi":"10.1007/s10337-026-04490-3","DOIUrl":"10.1007/s10337-026-04490-3","url":null,"abstract":"","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 4","pages":"491 - 491"},"PeriodicalIF":1.3,"publicationDate":"2026-03-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148237207","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Validation of the RP-HPLC Technique and Assessment of Uncertainty for the Hexaconazole Fungicide Residues in Tomato: A Sustainable Approach","authors":"Tanya Bisht,&nbsp;Anjana Srivastava,&nbsp;Gajanpal Singh","doi":"10.1007/s10337-026-04487-y","DOIUrl":"10.1007/s10337-026-04487-y","url":null,"abstract":"<div><p>An effective and straightforward analytical technique has been developed and validated for the quantification of hexaconazole fungicide used to manage fungal diseases on tomato crops. The measurement uncertainty was determined, and the environmental impact of the validated method was also assessed. The extraction of fungicide residues from tomato samples was performed using a modified QuEChERS method, followed by analysis via HPLC-UV. The validation parameters of the method, including specificity, linearity, matrix effects, limit of detection, limit of quantification, recovery, accuracy, precision, robustness, estimation of measurement uncertainty, and environmental impact, were assessed. The method’s specificity, determined by the purity of chromatographic peaks, was evident in the chromatograms of hexaconazole. The calibration curve exhibited linearity with an <i>R</i>² value &gt; 0.99. The matrix effect for the fungicide in tomato crops was found to be less than ± 20%, and the average recovery of hexaconazole at three different concentrations (LOQ, 5, and 10 LOQs) ranged from 84.69 to 93.29%, with a percent relative standard deviation of less than 4%. The combined uncertainty (Uc) was below the 25% default threshold, which is deemed acceptable for non-fatty matrices. The environmental impact of the method assessed using the Agro Eco Scale was found to be satisfactory. Thus, method validation for hexaconazole in tomatoes was achieved with high accuracy and sensitivity while minimizing the use of organic solvents. The developed approach is quick, affordable, and trustworthy, making it suitable for commercial testing, even in laboratories without access to expensive equipment.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 4","pages":"469 - 478"},"PeriodicalIF":1.3,"publicationDate":"2026-03-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148237189","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Identification of Volatiles and Non-volatiles Compounds and Quantification of Four Bioactive-Related Lipid Components in Supercritical CO2 Extract of Amorphophallus konjac Flying Powder","authors":"Xiaoyan Peng,&nbsp;Tao Zou,&nbsp;Xiaoyan Zou,&nbsp;Xiangheng Zeng,&nbsp;Caiyun Wang,&nbsp;Xue Zhou,&nbsp;Fahuan Ge","doi":"10.1007/s10337-026-04488-x","DOIUrl":"10.1007/s10337-026-04488-x","url":null,"abstract":"<div><p><i>Amorphophallus konjac</i>, as a plant with both medicinal and edible uses that is widely valued by people, the main research on it is still glucomannan. However, a large amount of byproduct—<i>Amorphophallus konjac</i> flying powder (AKFP)—is discarded during the refining process. The reason for this lies in the insufficient research on the bioactive compounds and quality contained in AKFP. In this study, two qualitative methods, ultra-performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS) and gas chromatography–mass spectrometry (GC–MS), were adopted to characterize the nonvolatile and volatile components in the supercritical CO₂ extract of AKFP (AKFPSE), and the contents of the four target components contained therein were determined by ultra-performance liquid chromatography–quadrupole/electrostatic field orbital trap high-resolution mass spectrometry (UPLC-Q-Exactive/MS). As a result, a total of 49 nonvolatile components and 35 volatile components were identified from the AKFPSE. In addition, the contents of <i>N</i>-hexanoyl-<span>D</span>-sphingosine (C6-SG) and <i>N</i>-acetyl dihydrosphingosine (C2-DSG) in the extract were determined to be 0.071 mg/g and 0.010 mg/g, respectively, and the contents of lysophosphatidylcholine 18:0 (LPC 18:0) and phosphatidylcholine 34:2 (PC 34:2) were 0.056 mg/g and 13.749 mg/g, respectively. In conclusion, this study employed highly sensitive mass spectrometry technology to comprehensively investigate the chemical composition and the content of nutritional components of AKFP from both qualitative and quantitative perspectives. This research can provide a research basis for the resource utilization and in-depth development of AKFP, and also offer a reference for the detection of lipids from other plant sources.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 4","pages":"479 - 489"},"PeriodicalIF":1.3,"publicationDate":"2026-03-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148237314","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Correlating Cell Partition Index and Thermodynamic Approaches to Study Biomass Adhesion onto Chromatographic Beads","authors":"Ajab Khan,&nbsp;Taiba Roedar,&nbsp;Muhammad Aasim,&nbsp;Hizb Ullah,&nbsp;Haris Saddique,&nbsp;Ibrar Ul Haq","doi":"10.1007/s10337-026-04486-z","DOIUrl":"10.1007/s10337-026-04486-z","url":null,"abstract":"<div><p>Biomass adsorption onto surfaces has a considerable role in many fields including biological science, drug innovation, ecological engineering, separation sciences, and the medical industry. The current research is sought to explore the interactions of microbial cells (undesirable) and proteins (desirable) with chromatographic beads by employing theoretical and experimental frameworks. The extended DLVO approach was used to analyze the interaction energies, while the cell partition index (CPI) technique was used for experimental validations. The aim of this study was to better understand the adhesion of cells and propose a simplified and cost-effective strategy for protein purification in adsorption chromatography. The results of this proposed framework revealed that salt concentration influences the interaction of cells or proteins with chromatographic beads. In hydrophobic interaction chromatography, CPI values decreased with increasing salt concentration, leading to enhanced secondary energy minimum between cells or proteins and Toyopearl Phenyl 650C beads. This effect was attributed to the exposure of hydrophobic patches, which promoted attractive forces between the interacting bodies. In contrast, during ion exchange chromatography, the CPI value increased with increased salt (NaCl) concentration, resulting in reduced interactions between cells/proteins with Toyopearl SP beads. This decrease was due to electrostatic screening and charge repulsion. These trends were consistent with calculated secondary interaction energy values obtained from xDLVO calculations. This research can assist in developing cost-effective and less complicated integrative technology, xDLVO-CPI approach, for understanding the interaction behavior. These findings may contribute to the development of less complex and more economical system for the purification of commercially important biomolecules from unclarified feedstock.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 4","pages":"455 - 467"},"PeriodicalIF":1.3,"publicationDate":"2026-03-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148236741","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Chemoselective Probes for Profiling of Carboxylic Acid Metabolites in Biological Tissue","authors":"Meng Wang,&nbsp;Renjun Zhang,&nbsp;Lulu Shang,&nbsp;Jingzhen Zhang,&nbsp;Liwei Wang,&nbsp;Mo Zhang","doi":"10.1007/s10337-026-04485-0","DOIUrl":"10.1007/s10337-026-04485-0","url":null,"abstract":"<div><p>Comprehensive profiling of carboxyl metabolites (CMs) is critical for biomarker discovery in disease pathogenesis but remains challenging due to matrix interference and poor ionization in mass spectrometry (MS). To overcome these limitations, we developed APH (amino-terminated polyuria–magnetic hexamethylenediamine composite), an integrated chemoselective probe for superior separation and detection. APH combines a magnetic Fe₃O₄@SiO₂ core for rapid isolation, a functionalized polyurea shell with high-density binding sites, a chemoselective moiety for covalent CMs capture, and a cleavable linker incorporating an MS signal-enhancing tag. This design enables specific enrichment of CMs directly from complex biosamples and efficient matrix removal via magnetic separation and gentle analyte release. Applied to mouse cecum samples, APH demonstrated deep carboxyl sub-metabolome profiling capabilities. By effectively reducing matrix suppression and enhancing sensitivity, APH facilitates the annotation of low-abundance CM biomarkers previously obscured in conventional analyses. This platform advances separation science for targeted metabolomics in biomarker research.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 4","pages":"443 - 453"},"PeriodicalIF":1.3,"publicationDate":"2026-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147878806","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Simply Preparation of Monodisperse SiO2 with the Effects of Inorganic Salts, Surfactants and their Assessment in Liquid Chromatography Applications","authors":"Xingyun Zhao,&nbsp;Xiaojian Liu,&nbsp;Zhenwei Zhang,&nbsp;Jiangyan Jin,&nbsp;Siyu Yang,&nbsp;Chengxiao Zhao,&nbsp;Rongfang Wu,&nbsp;Liyun Zhang","doi":"10.1007/s10337-026-04484-1","DOIUrl":"10.1007/s10337-026-04484-1","url":null,"abstract":"<div><p>Mesoporous silica particles were synthesized via investigating polymerization-induced colloidal aggregation (PICA) reaction process in our laboratory. Mesoporous microspheres with a particle size of about 2~7 μm and various surface morphology were first compared via varying the pH and molar ratio of formaldehyde/urea in the PICA process. The effects of salts and surfactant on the preparation were further investigated by fixing pH and molar ratio formaldehyde/urea (1:1.5), demonstrated that the particle size distribution became narrower when potassium sulphate and a nonionic surfactant were added together. The morphology, pore size distribution and the specific surface area of the synthesized mesoporous SiO₂ microspheres were observed and characterized by optical microscope, scanning electron microscope (SEM), dynamic light scattering (DLS), and specific surface area (BET) analysis. In the present study, synthesized materials modified octadecyltrichlorosilane (PICA-3@C18) were slurry-packed into a chromatographic empty column, resulting in successful separation of nonpolar compounds. Furthermore, the synthesized materials were functionalized with aminopropyl trimethoxysilane under optimized conditions and exhibited outstanding separation abilities. Aminopropyl trimethoxysilane was further bonded onto commercial SiO₂, resulting in a stationary phase that exhibited better chromatographic performance than commercial amide columns, NH₂ columns, and other HILIC columns. This work provides insight into retention behavior in HILIC mode and offers a foundation for the development of other amine-based HILIC stationary phases.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 4","pages":"431 - 441"},"PeriodicalIF":1.3,"publicationDate":"2026-02-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148237198","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Pesticide Residue Analysis and Health Risk Assessment in Vegetables from Conventional Farms in Cameron Highlands, Malaysia","authors":"Nusrat Bibi,&nbsp;Humaira Razaq,&nbsp;Nurfaizah Abu Tahrim","doi":"10.1007/s10337-026-04483-2","DOIUrl":"10.1007/s10337-026-04483-2","url":null,"abstract":"<div><p>The current study determines 15 pesticide residues of organochlorine (OCPs), organophosphorus pesticides (OPPs) and pyrethroids (PYRs) in vegetables from agricultural farms in Cameron Highlands, Malaysia, and evaluates the associated health risks. More than 200 vegetable samples were analysed during the wet season (October–January) and dry season (April–July). A multi-residue method was developed for the analysis of pesticides followed by gas chromatography (GC) in combination with an electron-capture detector (ECD). The average recovery was between 60% and 128%, while the relative standard deviation, RSD, was in the range of 0.2%–19.8%. The method validation was conducted by the external standard calibration. The highest concentrations were found in the wet season (5 μg/kg–100 μg/kg), possibly due to air circulation and greater pesticide usage by farmers. Overall, the concentrations ranged from 0.03 μg/kg to 100 μg/kg. Cabbage showed the highest concentration of each pesticide and thus was found to be the most contaminated vegetable amongst other vegetables of the region. The highest combined risk in brassica vegetables for children suggests that children might experience serious adverse health effects. Multivariate analysis shows that farmers are using a mixture of pesticides on vegetables and signifies the importance of pesticides application on crop type.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 4","pages":"419 - 429"},"PeriodicalIF":1.3,"publicationDate":"2026-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148237338","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"The Use of SEC-IR for Modeling and Calibrating the Comonomer Content from the 2D-LC Analysis Across the Molar Mass Distributions of LLDPE Samples","authors":"Paul DesLauriers,&nbsp;Jan-Hendrik Arndt,&nbsp;Guru Geertz,&nbsp;Subrajeet Deshmukh,&nbsp;Robert Brüll","doi":"10.1007/s10337-026-04481-4","DOIUrl":"10.1007/s10337-026-04481-4","url":null,"abstract":"<div><p>Solvent gradient interaction chromatography (SGIC) coupled to size exclusion chromatography (SEC), commonly referred to as 2D-LC, typically provides Three-dimensional data. Represented as contour plots, one axis shows the variation in molar mass (MM), and the other axis shows the comonomer (CM) content, while the detector intensity is color-coded. Currently, however, the accuracy of these systems is limited and provides only a qualitative understanding of these plots. In our previous work, we developed a single-sample integral calibration (SSIC) to mitigate current limitations and improve the accuracy of the molar mass measurements for metallocene-catalyzed polyethylene (mPE). In this current work, we addressed converting SGIC elution volumes (EV) to comonomer content across the molar mass distribution (MMD) of mPE samples using SEC-IR5 data as the calibrant.</p><p>Our results showed that a linear calibration of the SGIC EV axis can be achieved for a single sample using 2D-LC data acquired for the whole polymer, independent of branch type, CM content, or skewness of the CM distribution (CMD). Moreover, the same methodology was used to calibrate the CM content at each MM slice (and concurrently for each SGIC fraction) for the 2D-LC analysis of a 1-butene mPE copolymer. Furthermore, we showed that the resulting contour plot was successfully calibrated to &lt; 0.5 mol% CM content for &gt; 95% of the MMD, and numerical matrix data had an estimated quantitation limit for MM (<i>z</i> axis) of ~ 2 wt.%. Using these calibration methods now allows us to evaluate 2D-LC data using statistical methods to better understand the SGIC separation process and to predict physical properties.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 4","pages":"387 - 404"},"PeriodicalIF":1.3,"publicationDate":"2026-02-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148236645","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Analytical Green and White HPLC Method for the Quantification of Nitroso Impurities in Darolutamide with MS/MS Characterization and In silico Toxicity Assessment of Degradation Products","authors":"Katari Ravi Babu,&nbsp;Gowri Sankar Reddipalli","doi":"10.1007/s10337-026-04476-1","DOIUrl":"10.1007/s10337-026-04476-1","url":null,"abstract":"<div><p>The present study describes the development of a green, stability-indicating HPLC method coupled with LC–MS/MS characterization for degradation products (DPs) of darolutamide. The chromatographic separation was achieved on a phenyl-hexyl column (250 × 4.6 mm, 5 µm) using an isocratic mobile phase of ethanol and 5 mM ammonium formate with 0.1% formic acid (55:45, v/v, pH 3.6) at 0.8 mL/min, with UV detection at 238 nm. The method provides sharp, symmetrical peaks with retention times of 5.8 min, 4.2 min, 1.59 min, and 2.96 min for darolutamide, nitroso impurity, and nitroso impurities 1 and 2. The forced degradation studies reveal that darolutamide was most susceptible to acid, base, and oxidative stress. These stress degradation lead to the formation of six novel DPs (DP1-DP6). The structural elucidation by LC–MS/MS confirms that DP1 and DP2 were nitrile hydrolysis products (amide and carboxylic acid derivatives). The DP3 was arising from alcohol oxidation to ketone, whereas DP6 results from acid-catalyzed dehydration to an alkene. The DP4 and DP5 emerge from sequential amide bond cleavage and side-chain loss from the darolutamide. The in silico toxicity prediction classifies all DPs in toxicity classes 4–5 (LD₅₀ = 1000–2200 mg/kg), with low acute toxicity. The method validation confirms the excellent linearity (r² &gt; 0.996), high precision (%RSD &lt; 1.0%), accuracy (recoveries 99.4–101.1%), robustness, and sensitivity (LOD as low as 0.015 µg/mL). The method’s greenness and sustainability were proved with an AGREE score of 0.83, ComplexGAPI, and an RGB whiteness score of 80.1%. This study highlights the compliance of the method with green and white analytical chemistry. This work uniquely addresses the nitroso impurities of regulatory concern with superior environmental and analytical performance. In conclusion, the proposed method was a sustainable, reliable, and regulatory-compliant approach for routine impurity profiling and stability assessment of darolutamide.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 4","pages":"357 - 372"},"PeriodicalIF":1.3,"publicationDate":"2026-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148236594","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Insight into the Retention Behaviours of Proton Pump Inhibitor Drugs Using Homemade ZIC-HILIC Columns with Greenness, Whiteness, and Blueness Evaluation","authors":"Mustafa J. Mohammed,&nbsp;Ashraf Saad Rasheed,&nbsp;Bashar Qasim","doi":"10.1007/s10337-026-04478-z","DOIUrl":"10.1007/s10337-026-04478-z","url":null,"abstract":"<div><p>In the current investigation, the chromatographic behavior of two homemade ZIC-HILIC stationary phases with different spacer chains between the ionic site groups, the ZIC-1 and ZIC-4, under aqueous mobile phase conditions is presented. As test compounds, two proton pump inhibitors (PPIs) were chosen. The effect of different spacer lengths on the retention behaviors of esomeprazole and lansoprazole was examined. The development process included investigating the impacts of chromatographic parameters, such as the ratio of organic modifier to aqueous buffer, pH values, the ionic strength of the acetate buffer, and experimental evaluation of the principal retention mechanism. The chromatographic separation was conducted using two zwitterionic columns measuring (100 mm × 4.6 mm, 3.5 µm particle size). The mobile phase consisted of a combination of acetonitrile and acetate buffer at a pH of 4.75 and ionic strength of 40 mM, in a ratio of 80:20 (<i>v</i>/<i>v</i>). The elution was performed using a constant flow rate of 0.5 mL min⁻¹. Detection was performed using a UV detector at a wavelength of 285 nm. The findings showed that increasing the spacer chain length causes an increase in the retention time for both analytes. The technique indicates excellent linearity, low detection limits, and high precision, and it was successfully applied to the determination of two analytes in pharmaceutical preparations with recovery values of 98–101%. Five of the most well-known metrics for evaluating the greenness of chemical methods were examined. Amongst these, AES, AGREE, NAMI, BAGI, and GAPI emerged as reliable tools for the assessment of greenness.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 3","pages":"345 - 356"},"PeriodicalIF":1.3,"publicationDate":"2026-02-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147621101","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}