Chromatographia最新文献_第2页

Sustainable Stability Analysis of Vibegron: A Novel Chromatographic Method Development and Validation Vibegron的可持续稳定性分析：一种新的色谱方法的开发和验证

IF 1.3 4区化学

Chromatographia Pub Date : 2025-08-18 DOI: 10.1007/s10337-025-04430-7

Nidhi Vadnere, Mital Patel

{"title":"Sustainable Stability Analysis of Vibegron: A Novel Chromatographic Method Development and Validation","authors":"Nidhi Vadnere, Mital Patel","doi":"10.1007/s10337-025-04430-7","DOIUrl":"10.1007/s10337-025-04430-7","url":null,"abstract":"<div><p>A stability-indicating high-performance liquid chromatographic (HPLC) method for Vibegron (VBG) was developed and validated based on the analytical quality-by-design (AQbD) concept. Screening of critical factors were studied using risk assessment, followed by Plackett–Burman design, and optimization of critical factors were done using an I-optimal response surface design. The optimized chromatographic conditions include a Kromasil Classic C18 column (250 × 4.6 mm, 5 µm) and a mobile phase consisting of acetonitrile (A) and 10 mM ammonium acetate buffer pH adjusted to 4.5 with trifluoroacetic acid (B); in a ratio of (A:B; 46:54 v/v) ratio, at a flow rate of 0.8 mL/min, with a detection wavelength of 248 nm. The method has been validated as per ICH guidelines and demonstrated linearity (<i>R</i><sup>2</sup> > 0.997), precision (% RSD < 2), and accuracy (99.97 ± 1.61% recovery). VBG was found to be sensitive during stress testing under various environmental conditions, including hydrolytic, oxidative, thermal, and photolytic stress. A total of 18 degradation products were separated, identified, and quantified using the developed method. The method's sustainability was assessed using the Whiteness assessment via the RGB 12 algorithm, the Analytical GREEness Tool (AGREE), the Complex Green Analytical Procedure Index, and the Blue Applicability Index, ultimately confirming that it is both green and practical. The developed method can be applied in pre-formulation studies, quality control, and pharmacovigilance.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 9","pages":"685 - 702"},"PeriodicalIF":1.3,"publicationDate":"2025-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145011670","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}

引用次数: 0

A Stability Indicating Reversed-Phase HPLC Method for Determination of Pyrantel and Its Related Substances in Commercial Bulk Batches of Pyrantel Pamoate 稳定性指示反相高效液相色谱法测定商业散装帕马酸吡喃酯中吡喃酯及其有关物质

IF 1.3 4区化学

Chromatographia Pub Date : 2025-08-18 DOI: 10.1007/s10337-025-04428-1

Mohammad Mosharraf Hossain, Abu M. Rustum

{"title":"A Stability Indicating Reversed-Phase HPLC Method for Determination of Pyrantel and Its Related Substances in Commercial Bulk Batches of Pyrantel Pamoate","authors":"Mohammad Mosharraf Hossain, Abu M. Rustum","doi":"10.1007/s10337-025-04428-1","DOIUrl":"10.1007/s10337-025-04428-1","url":null,"abstract":"<div><p>Pyrantel is used as an active pharmaceutical ingredient (API) in both human and veterinary drug products. It is widely available as pyrantel pamoate (PP) and is also referred to as pyrantel embonate. It acts as a depolarizing neuromuscular blocking agent, causing paralysis in parasitic worms (helminths). The objective of this work was to develop an efficient, selective, and robust reversed phase high-performance liquid chromatography (RP-HPLC) method to determine PP and its related impurities in bulk API batches. The new method utilizes a Waters Xselect®HSS T3 column (100 mm × 4.6 mm i.d., 2.5 μm particle size) at 30 °C, with 0.1% TFA in H2O as mobile phase A and 100% methanol as mobile phase B. Analytes were separated by gradient elution at a flow rate of 1.0 mL/min and were detected by UV at 280 nm, except for impurity D (at 215 nm). The total run time of the method is 18 minutes. Unlike the PP methods prescribed in USP and Ph. Eur., the new HPLC method described in this paper adequately separates all peaks of interest and have demonstrated excellent robustness and reproducibility across various varied conditions. The results of forced degradation studies confirmed its stability-indicating capability. The validation results demonstrated that the new method is accurate, robust, specific, and stability-indicating. One of the key strengths and highlight of the new method is its capability in resolving the co-eluting peaks under the conditions of the USP/Ph. Eur. Methods.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 9","pages":"673 - 683"},"PeriodicalIF":1.3,"publicationDate":"2025-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145011669","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}

引用次数: 0

Development of Ionic Liquid-Based Dispersive Liquid–Liquid Microextraction Assisted by Acetone-Based Salting-Out Extraction for Multiclass Pesticide Quantification in Tomato Using HPLC–DAD 离子液体分散液液微萃取辅助丙酮盐析萃取在番茄中多类农药定量分析中的应用

IF 1.3 4区化学

Chromatographia Pub Date : 2025-08-18 DOI: 10.1007/s10337-025-04433-4

Bezuayehu Tadesse Negussie, Simiso Dube, Mathew Muzi Nindi, Asmamaw Tesfaw

{"title":"Development of Ionic Liquid-Based Dispersive Liquid–Liquid Microextraction Assisted by Acetone-Based Salting-Out Extraction for Multiclass Pesticide Quantification in Tomato Using HPLC–DAD","authors":"Bezuayehu Tadesse Negussie, Simiso Dube, Mathew Muzi Nindi, Asmamaw Tesfaw","doi":"10.1007/s10337-025-04433-4","DOIUrl":"10.1007/s10337-025-04433-4","url":null,"abstract":"<div><p>An ionic liquid-based dispersive liquid–liquid microextraction (IL-DLLME) technique with low LODs, high enrichment factors, and reduced solvent use was devised for the extraction and determination of multiclass pesticide residues in tomato samples. The extraction process uses acetone for the initial extraction of pesticides from tomatoes, followed by dispersive liquid–liquid microextraction using 1-hexyl-3-methylimidazolium hexafluorophosphate as the extraction solvent. The critical parameters that affect the extraction efficiency, such as the type and volume of the extraction solvent, the volume of the dispersive solvent, the type and volume of the ionic liquid, pH, and salt addition, were meticulously optimized. Under these optimized conditions, the method exhibited robust linearity (R<sup>2</sup> ≥ 0.9960), low limits of detection (2.0–7.3 µg/kg) and quantification (5.6–19.4 µg/kg), along with satisfactory precision (RSD ≤ 10.4%) and recovery rates (88.0 to 105.3%) for the pesticides of interest. The proposed method represents a promising tool for routine pesticide monitoring in food quality control laboratories.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 9","pages":"703 - 715"},"PeriodicalIF":1.3,"publicationDate":"2025-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145011671","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}

引用次数: 0

Thermodynamics of Transport Phenomena in Field-Flow Fractionation: Organized Structures Formation 场流分馏中输运现象的热力学：有组织结构的形成

IF 1.3 4区化学

Chromatographia Pub Date : 2025-08-16 DOI: 10.1007/s10337-025-04422-7

Josef Janča

{"title":"Thermodynamics of Transport Phenomena in Field-Flow Fractionation: Organized Structures Formation","authors":"Josef Janča","doi":"10.1007/s10337-025-04422-7","DOIUrl":"10.1007/s10337-025-04422-7","url":null,"abstract":"<div><p>The classical theoretical model of the field-flow fractionation, assuming the exponential concentration distribution of the species affected by the external fields in polarization mechanism, is just an approximation neglecting the possible formation of the organized structures. Original use of Riemann’s integral to calculate the dimensionless exponential concentration distribution enables to study the thermodynamic aspects and the related transport phenomena for model systems where the field forces are weak and to obtain precise and predictive results on the equilibrium positions of the species forming the focused zones by two different mechanisms. The samples injected into the separation units of the field-flow fractionation are rather diluted but the applied field forces transport the macromolecular or particulate species and produce the zones of much higher concentration. Consequently, the organized structures, that constitute the spacially oriented concentration gradients in the direction of the effective field forces, appropriate to each particular separation mechanism, may appear whenever the repulsive interactions among the dissolved or dispersed species restrict their free Brownian motion. It is difficult to detect the existence of such structures directly in thin field-flow fractionation channels but it was unquestionably proven by the small angle X-ray scattering of larger volume of the negatively charged nanometer sized particles in aqueous suspension of silica. The experimental equilibrium positions of the particles of different densities but almost the same size, focused by the action of lift forces, were identical, but their trajectories from the starting takeoff from the accumulation wall to the equilibrium positions were different. This finding inspired the idea to exploit this effect for rapid focusing micro-TFFF.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 9","pages":"659 - 671"},"PeriodicalIF":1.3,"publicationDate":"2025-08-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-025-04422-7.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145011452","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"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

Characterization and Establishment of Validated Reverse-Phase HPLC Method for Bergapten-Loaded Nanostructured Lipid Carriers 载bergap苷纳米脂质载体的表征及反相高效液相色谱方法的建立

IF 1.3 4区化学

Chromatographia Pub Date : 2025-08-04 DOI: 10.1007/s10337-025-04425-4

Muneeb Ur Rahman, Shumaila Arshad, Mulazim Hussain Asim, Alamgeer, Hafiz Muhammad Irfan, Nayab Tahir

{"title":"Characterization and Establishment of Validated Reverse-Phase HPLC Method for Bergapten-Loaded Nanostructured Lipid Carriers","authors":"Muneeb Ur Rahman, Shumaila Arshad, Mulazim Hussain Asim,  Alamgeer, Hafiz Muhammad Irfan, Nayab Tahir","doi":"10.1007/s10337-025-04425-4","DOIUrl":"10.1007/s10337-025-04425-4","url":null,"abstract":"<div><p>The purpose of the study was to synthesize bergapten-loaded nanostructured lipid carriers (NLCs) to characterize and develop an HPLC method. The bergapten-loaded NCLs were characterized for size, polydispersity index (PDI), and zeta potential (ZP). The morphology of NLCs was observed by scanning electron microscopy (SEM). The drug encapsulation and loading efficiency were evaluated. Moreover, an HPLC method was developed and validated in terms of accuracy, precision, specificity, linearity, limit of detection, and limit of quantitation. Bergapten-loaded NLCs exhibited a size of 23.5 nm with 0.25 PDI, confirming narrow size distributions, whereas blank NLCs showed 20.7 nm size and 0.19 PDI. The ZP of bergapten-loaded NLCs was − 13.0 mV, which was found to be almost the same as blank NLCs. SEM images confirmed the smooth surface and spherical shape of NLCs. The HPLC-validated method for drug quantification was found to be simple and efficient. Successful fabrication of drug-loaded NLCs showed size, PDI, and ZP within range with a smooth and spherical shape, and HPLC methods showed good estimation of bergapten in NLCs.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 8","pages":"625 - 635"},"PeriodicalIF":1.3,"publicationDate":"2025-08-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145037247","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}

引用次数: 0

Evolution, Uses, and Emerging Trends in Microfluidic Paper-Based Analytical Devices 微流控纸基分析装置的发展、用途和新兴趋势

IF 1.3 4区化学

Chromatographia Pub Date : 2025-07-31 DOI: 10.1007/s10337-025-04424-5

Chandrababu Rejeeth, Robin Kumar Pundir, Prachi Singhal, D. V. Surya Prakash

{"title":"Evolution, Uses, and Emerging Trends in Microfluidic Paper-Based Analytical Devices","authors":"Chandrababu Rejeeth, Robin Kumar Pundir, Prachi Singhal, D. V. Surya Prakash","doi":"10.1007/s10337-025-04424-5","DOIUrl":"10.1007/s10337-025-04424-5","url":null,"abstract":"<div><p>Microfluidic paper-based analytical devices (µPADs) are valued of their low cost and portability, making them perfect for testing at the point of need. Their adaptability in size and shape further improves their portability, detection and analysis that can be carried out with portable devices. µPADs meet the essential demand for quick, dependable and simple testing in diverse areas, such as environmental monitoring, healthcare and food safety. This review offers a thorough overview of the development of µPADs, exploring key design factors such as the type of paper utilized and the core operational principles. Key detection methods include colorimetry, fluorescence, and electrochemistry, with recent innovations combining optical and electrochemical techniques to improve sensitivity and selectivity. In addition, distance-based detection methods are emphasized for their ability to provide instrument-free analysis and minimize error, which is especially important in resource-limited settings. The review concludes by addressing the practical challenges and requirements of µPADs, providing valuable insights for future research and advancements in the field of analytical chemistry.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 8","pages":"531 - 554"},"PeriodicalIF":1.3,"publicationDate":"2025-07-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145037553","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}

引用次数: 0

Multivariate Optimization of Chloride Extraction from Commercial and Raw Diesel Oil for the Determination by Ion Chromatography 离子色谱法测定商品柴油和原料柴油中氯离子含量的多元优化

IF 1.3 4区化学

Chromatographia Pub Date : 2025-07-26 DOI: 10.1007/s10337-025-04423-6

Adriana Fernández-Campos, Alessandra R. Cassella, Ricardo J. Cassella

{"title":"Multivariate Optimization of Chloride Extraction from Commercial and Raw Diesel Oil for the Determination by Ion Chromatography","authors":"Adriana Fernández-Campos, Alessandra R. Cassella, Ricardo J. Cassella","doi":"10.1007/s10337-025-04423-6","DOIUrl":"10.1007/s10337-025-04423-6","url":null,"abstract":"<div><p>The determination of chloride in crude oil and its derivatives is a matter of utmost importance for the petroleum industry. In this study, we developed a straightforward methodology for chloride extraction for its determination in diesel oil. The extraction was performed using deionized water, employing microwave radiation as the energy source, and the quantification of chloride in the extracts was conducted by ion chromatography. The method was optimized using a multivariate approach through a Doehlert design. The optimized variables included sample mass (between 0.25 and 1.25 g), extraction time (between 5 and 35 min), and extraction temperature (between 100 and 150 °C). Only sample mass showed a significant effect on extraction efficiency, although the temperature used in the process could not exceed 150 °C to avoid sample degradation. Under the optimized conditions (0.25 g of sample in 10.00 mL of deionized water, maintained at 125 °C for 20 min), the limits of detection and quantification of the method were 0.24 µg g<sup>–1</sup> and 0.72 µg g<sup>–1</sup>, respectively. It was successfully applied for chloride determination in six samples of both commercial and raw diesel oil. An average recovery rate of 94 ± 10% was obtained in the recovery assays.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 8","pages":"615 - 624"},"PeriodicalIF":1.3,"publicationDate":"2025-07-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145037321","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}

引用次数: 0

Determination of Aripiprazole, Blonanserin, and Their Metabolites in Human Urine by Automated μSPE–LC–MS/MS 自动μSPE-LC-MS /MS法测定人尿中阿立哌唑、勃兰色林及其代谢物

IF 1.3 4区化学

Chromatographia Pub Date : 2025-07-04 DOI: 10.1007/s10337-025-04419-2

Yeong Eun Sim, Minyoul Kim, Jae-il Lee, Jin Young Kim

{"title":"Determination of Aripiprazole, Blonanserin, and Their Metabolites in Human Urine by Automated μSPE–LC–MS/MS","authors":"Yeong Eun Sim, Minyoul Kim, Jae-il Lee, Jin Young Kim","doi":"10.1007/s10337-025-04419-2","DOIUrl":"10.1007/s10337-025-04419-2","url":null,"abstract":"<div><p>In this study, an automated micro-solid-phase extraction (μSPE)–liquid chromatography–tandem mass spectrometric (LC–MS/MS) method was developed and validated to determine aripiprazole, dehydroaripiprazole, blonanserin, and N-desmethyl blonanserin in human urine. An instrument top sample preparation cartridge was implemented to enhance analyte sensitivity and mitigate the matrix effects from urine samples. LC–MS/MS analysis employed a multiple-reaction monitoring mode, with analyte separation achieved using a Capcell Pak C18 MGIII column (2.0 × 150 mm, 5 µm). The mobile phase comprised a 10 mM ammonium formate solution with 0.1% formic acid and acetonitrile. The calibration range for all analytes was 0.1–50 ng mL<sup>−1</sup>, yielding correlation coefficients (<i>r</i>) of ≥ 0.9993 and a weighting factor of 1/x<sup>2</sup>. The detection limits for all analytes were 0.03 ng mL<sup>−1</sup>. Intra- and inter-day accuracy ranged from − 3.6 to 5.0% and − 4.0 to 3.3%, respectively, with precision values of ≤ 9.5% and ≤ 12.9%. This validated method was successfully applied to 107 forensic urine samples. Urinary creatinine normalization was used to adjust analyte concentrations in urine. Normalized concentrations of aripiprazole, dehydroaripiprazole, blonanserin, and N-desethyl blonanserin were detected at 0.1–185.2 (n = 86), 0.2–295.5 (n = 91), 0.1–0.7 (n = 7), and 0.2–1.6 (n = 12) ng mg<sup>−1</sup> creatinine, respectively.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 8","pages":"595 - 613"},"PeriodicalIF":1.3,"publicationDate":"2025-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145037267","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}

引用次数: 0

Green Analytical HPLC Method Development for Impurity Profiling of Ivosidenib with LCMS/MS Characterization and In Silico Toxicity Prediction of its Degradation Products 绿色高效液相色谱法建立依沃西替尼杂质谱分析及降解产物的硅毒性预测

IF 1.3 4区化学

Chromatographia Pub Date : 2025-06-26 DOI: 10.1007/s10337-025-04420-9

Sateesh Reddy Vuyyuru, Noura Sultan Al Shamsi, Kota Thirumala Prasad, A. Venkateswara Rao

{"title":"Green Analytical HPLC Method Development for Impurity Profiling of Ivosidenib with LCMS/MS Characterization and In Silico Toxicity Prediction of its Degradation Products","authors":"Sateesh Reddy Vuyyuru, Noura Sultan Al Shamsi, Kota Thirumala Prasad, A. Venkateswara Rao","doi":"10.1007/s10337-025-04420-9","DOIUrl":"10.1007/s10337-025-04420-9","url":null,"abstract":"<div><p>The study aimed to optimize and validate a robust green HPLC method for quantifying and separating process-related impurities of ivosidenib. Further, the study intended to characterize the degradation products (DPs) of ivosidenib formed under various stress conditions. Among the columns tested, the Zorbax Eclipse Plus C18 column (250 mm) column was proved to be the best for the resolution of ivosidenib and its impurities using ethanol and 0.1% aqueous formic acid in 45:55 (v/v) at 0.8 mL/min flow rate and 245 nm detector wavelength. This method produces a clear resolution of ivosidenib and its impurities with no interference from blank samples providing the specificity and robustness of the method. The technique demonstrated linearity (<i>r</i><sup>2</sup> ≥ 0.9994), precision (intraday and interday % RSD < 2), accuracy (recovery: 98–102%), ruggedness, robustness, and stability under varied conditions. Forced degradation studies revealed distinct DPs under acidic, UV, and oxidative stress conditions, and these DPs were characterized using LC–MS techniques. The toxicity prediction indicated neurotoxicity and respiratory toxicity for all DPs with specific compounds exhibiting hepatotoxicity, nephrotoxicity, or immunotoxicity. The environmental impact of the proposed method was assessed through AGREE and GAPI tools and the technique exhibits high compliance with green analytical chemistry principles. This result highlights method reliability, efficiency, and eco-friendliness to pharmaceutical safety and environmental sustainability.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 8","pages":"583 - 594"},"PeriodicalIF":1.3,"publicationDate":"2025-06-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145037389","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}

引用次数: 0

Quantitative Assessment of 2D-LC Analysis of Polyolefins for Multiway Applications: Calibration of the Log M Axis 用于多路应用的2D-LC分析聚烯烃的定量评估：对数M轴的校准

IF 1.3 4区化学

Chromatographia Pub Date : 2025-06-26 DOI: 10.1007/s10337-025-04413-8

Paul DesLauriers, Jan-Hendrik Arndt, Guru Geertz, Subrajeet Deshmukh, Robert Brüll

{"title":"Quantitative Assessment of 2D-LC Analysis of Polyolefins for Multiway Applications: Calibration of the Log M Axis","authors":"Paul DesLauriers, Jan-Hendrik Arndt, Guru Geertz, Subrajeet Deshmukh, Robert Brüll","doi":"10.1007/s10337-025-04413-8","DOIUrl":"10.1007/s10337-025-04413-8","url":null,"abstract":"<div><p>Two-dimensional high performance liquid chromatography (2D-LC) offers unique insights into the polyolefins’ chemical composition and how that relates to their molar mass distribution. Moreover, the numerical format of the sample’s 2D-LC data (i.e., the <i>J x K</i> matrix of molar mass (MM) and comonomer (CM) content, respectively) allows for further correlations between the sample’s structural parameters and its physical properties via statistical multi-way methods. However, before applying these advanced methods to multi-sample data sets, we first determined the extent of variability and quantitation limits of these structural parameters for individual samples. In this current work we evaluated the 2D-LC MM data (measured on one SEC column) for a number of metallocene-catalyzed polyethylene resins and compared the results to those acquired on a typical three column SEC unit.</p><p>Our initial assessment shows that the presence of 1-decanol interferes with accurate MM measurements when using typical calibration methods that employ MHS constants. However, accurate MM data were obtained by using a single sample integral calibration (SSIC) method, where the sample’s MMD measured on a three-column SEC unit is used to calibrate the 2D-LC SEC data. The resulting MM values were within the expected error and consistent with published data. Additionally, the resulting MMD profiles, coupled with the known short-chain branching content for the samples, gave the expected crystallinity properties as measured by DSC and estimated densities.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 8","pages":"563 - 581"},"PeriodicalIF":1.3,"publicationDate":"2025-06-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-025-04413-8.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145037322","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"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