Chromatographia最新文献

{"title":"Construction and Application of a Novel Universal Detection System for High Performance Capillary Electrophoresis","authors":"Tao Huang,&nbsp;Chunsu Liang,&nbsp;Jing Li,&nbsp;Liyu Gong,&nbsp;Jinxiang Xu,&nbsp;Kai Zhu,&nbsp;Xibei Yang,&nbsp;Xin Hu,&nbsp;Youqi Yan,&nbsp;Xiaomei Ling","doi":"10.1007/s10337-024-04320-4","DOIUrl":"10.1007/s10337-024-04320-4","url":null,"abstract":"<div><p>Conventional high performance capillary electrophoresis (HPCE) detection modes mainly rely on chromogenic, fluorogenic, ionizable, or redox properties of analytes, greatly limiting the scope of analysis. Therefore, the development of a universal HPCE detection system has raised great attention. Herein, by tandem connection of different diameter capillaries (TCDDC), a novel and universal HPCE detection system called interface-induced current detector (IICRD) was constructed. The current signal peaks of analytes in the current-electrophoretograms (CR-EGs) can be observed for the first time. The results of detector performance tests showed good repeatability and high sensitivity. The theoretical deduction and experimental verification were further carried out. To prove the detection ability, several substances with or without special responsive groups were qualitatively and quantitatively analyzed. Firstly, cations and anions in inorganic electrolytes (inorganic salts, acids and alkalis) can be simultaneously separated and analyzed. Furthermore, several small molecular weight organic compounds, monosaccharides and disaccharides were also analyzed. The current signal peaks in CR-EGs were identified and discussed. For quantitative analysis, system suitability tests were evaluated, the results of quantitative analysis methodology validation showed that the new method was qualified for quantitative analysis. The linear relationship between the values of current intensity and the concentrations of analytes can be obtained over the investigated concentration ranges. In summary, the HPCE-DAD-IICRD system showed lower baseline noise, higher sensitivity and higher S/N especially for samples without special responsive groups, showing complementary advantages when combined with other detectors. It is expected to be a novel HPCE detection system for extensive applications.</p><h3>Graphical Abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 5","pages":"325 - 337"},"PeriodicalIF":1.2,"publicationDate":"2024-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140313697","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":"Comprehensive Stress Degradation Studies of Fipronil: Identification and Characterization of Major Degradation Products of Fipronil Including Their Degradation Pathways Using High Resolution-LCMS","authors":"Shane N. Berger,&nbsp;Abu M. Rustum","doi":"10.1007/s10337-024-04324-0","DOIUrl":"10.1007/s10337-024-04324-0","url":null,"abstract":"<div><p>Fipronil belongs to the phenylpyrazole family of insecticides and functions by interrupting the γ-aminobutyric acid system and chloride ion channels of pests. Studies have shown Fipronil can undergo several degradation pathways in the environment to form degradants that may be toxic to non-target aquatic life. In this study, a comprehensive forced degradation study of Fipronil was carried out following ICH guidelines to generate, characterize, and identify the major degradation products of Fipronil. Stress conditions included acidic, alkaline, oxidative, thermal (solid and solution states), and photolytic (solid and solution states). Separation of six major degradation products (DPs) was achieved using reversed phase high-performance liquid chromatography (HPLC) with gradient elution. The DPs were characterized and identified using HPLC-high-resolution mass spectrometry (HPLC-HRMS) and comparison of tandem MS/MS fragmentation profiles. The Fipronil dimer required isolation through semi-preparative HPLC and analysis by nuclear magnetic resonance (NMR) to elucidate and confirm its structure. The proposed structures of DPs were based upon the given degradation pathways of Fipronil. The key results and findings of this study will provide better understanding of Fipronil stability and its major degradation products including degradation/formation pathways, which would assist designing of more stable Fipronil formulations and finished products with extended shelf-life including enhanced efficacy with decreased adverse effects.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 4","pages":"249 - 257"},"PeriodicalIF":1.2,"publicationDate":"2024-03-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140128384","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":"Women in Science Now: Stories and Strategies for Achieving Equity","authors":"Claudia Zielke","doi":"10.1007/s10337-024-04327-x","DOIUrl":"10.1007/s10337-024-04327-x","url":null,"abstract":"","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 4","pages":"269 - 271"},"PeriodicalIF":1.2,"publicationDate":"2024-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140253717","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":"Focusing Mechanisms in Micro-thermal Field-Flow Fractionation","authors":"Josef Janča","doi":"10.1007/s10337-024-04316-0","DOIUrl":"10.1007/s10337-024-04316-0","url":null,"abstract":"<div><p>Progress in theory of separation mechanisms controlling the Micro-Thermal Field-Flow Fractionation of the macromolecular and particulate species inspired the development of the experimental methodology and instrumental techniques. Three really functioning separation mechanisms are polarization, steric and focusing. However, steric mechanism is rather exceptionally operative for the separation of large particles at low flow rates of the carrier liquid. On the other hand, two <i>modus operandi</i> taking advantage of focusing mechanism emerging at high flow rates and, consequently, resulting in very rapid separations are elaborated. One exploits the action of the lift force and the other one makes use of the kinetic energy generated by the collisions among the particles in bi-disperse suspension of the particulate species. Surface properties and their topographical heterogeneity influence the migration of particulate species exposed to the force of thermal diffusion. The shape of the spherical versus non-spherical particles distinguishes their behavior when exposed to thermal diffusion and to hydrodynamic stress. It was theoretically calculated that the separations of the particles, based on the mentioned differences, are possible by Focusing Micro-Thermal Field-Flow Fractionation. Since our earlier theoretical models were not developed in sufficient details, some of the previous results are corrected by the present paper. The theoretical conclusions are supported by preceding real separations.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 4","pages":"259 - 268"},"PeriodicalIF":1.2,"publicationDate":"2024-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140099042","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":"Congress, Conferences, and Workshops","authors":"","doi":"10.1007/s10337-024-04322-2","DOIUrl":"10.1007/s10337-024-04322-2","url":null,"abstract":"","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 4","pages":"273 - 274"},"PeriodicalIF":1.2,"publicationDate":"2024-02-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142414162","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":"Characterization of Elvitegravir and Its Related Impurities Using ESI–LC–MS, NMR Techniques, Method Development and Validation of Its Related Substances by HPLC Method","authors":"Sambandan Elumalai,&nbsp;Sellappan Senthilkumar,&nbsp;Mamidala Srikanth,&nbsp;Venkata Bharat Nishtala,&nbsp;Kathavarayan Thenmozhi","doi":"10.1007/s10337-024-04314-2","DOIUrl":"10.1007/s10337-024-04314-2","url":null,"abstract":"<div><p>Elvitegravir (ETV), drug substance, and its eleven process-related impurities have been identified and their structural identification study has been carried out with the aid of ¹H, ¹³C NMR, and ESI–LC–MS spectroscopic techniques. Plausible fragments were also proposed for each impurity to ascertain its structure. Simple, facile, and selective, stability indicating, mass spectrometry compatible HPLC method has been developed and subsequently validated with the validation parameters of specificity, LOD, LOQ, precision at LOQ, linearity, accuracy at LOQ to 120% levels, method precision, intermediate precision studies, and solution stability has also been established. This method encompasses a simple gradient mode of separation with mobile phases—(A) 0.1% trifluoroacetic acid in water and (B) 0.1% trifluoroacetic acid in acetonitrile, the mass sectrometric compatible mobile phase has been chosen for the identification of known, unknown and degradation impurities. To assess the nature of each impurity, whether they are either process-related or degradation-induced, an intensive stress study has also been conducted. From this degradation assessment, all the impurities have been classified as process-related. Further, the assessment of three different manufacturers samples was also executed to show the method applicability and comparison of quality of the different manufacturers drug, and thus this method shall be engaged as a quality inferring tool for the marketed sample.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 4","pages":"227 - 248"},"PeriodicalIF":1.2,"publicationDate":"2024-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139924764","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":"Quantification of Residual Organic Solvents in Clobetasol Propionate using Headspace Capillary Gas Chromatography","authors":"Xiaoyi Shi,&nbsp;Shuai Li,&nbsp;Zhao Li,&nbsp;Hangri Zeng,&nbsp;Yi Liu,&nbsp;Wen Lan,&nbsp;Yanming Liu,&nbsp;Jinfeng Zheng","doi":"10.1007/s10337-024-04313-3","DOIUrl":"10.1007/s10337-024-04313-3","url":null,"abstract":"<div><h3>Objective</h3><p>In this study, we aimed to develop a headspace capillary gas chromatography method to quantify residual methanol, acetone, methylene chloride, diisopropyl ether, ethyl acetate, and n,n-dimethylformamide (DMF), in raw clobetasol propionate.</p><h3>Methods</h3><p>The headspace gas chromatography method employs a chromatographic column packed with 6% cyanopropylphenyl-94% dimethylpolysiloxane as the stationary phase. The column temperature program initiated at 40 °C, was held for 10 min, then ramped up at 10 °C per minute to 220 °C, and maintained for 1 min. Nitrogen served as the carrier gas at a flow rate of 4.84 ml/min. The injection port temperature was set at 140 °C; the flame ionization detector (FID) operated at 250 °C, and the headspace equilibrium temperature was maintained at 105 °C with a 30 min equilibration time.</p><h3>Results</h3><p>All six residual solvents exhibited complete separation, displaying strong linearity and achieving high recovery rates. Furthermore, the residual solvent levels in the six samples tested remained comfortably below the permissible limit.</p><h3>Conclusion</h3><p>Our method is accurate, reliable, rapid, and sensitive, making it well-suited for the detection of organic residual solvents in raw clobetasol propionate.</p><h3>Graphical Abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 4","pages":"195 - 202"},"PeriodicalIF":1.2,"publicationDate":"2024-02-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139924789","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":"Development of RP-HPLC–UV Technique for “N,N’-Disubstituted Terephthalamides”, the Depolymerized End Products of Polyethylene Terephthalate Waste","authors":"Shifa Altaf,&nbsp;Meenu Teotia,&nbsp;R. K. Soni","doi":"10.1007/s10337-024-04321-3","DOIUrl":"10.1007/s10337-024-04321-3","url":null,"abstract":"<div><p>Amides often exhibit poor solubility in common solvents, posing challenges to their efficient separation. However, the development of robust RP-HPLC methods becomes essential to overcome this limitation, enabling accurate and reliable separation, quantification and characterization of these compounds. An RP-HPLC–UV technique has been developed for evaluating N,N’-dibutylterephthalamide, N,N’-dimethylterephthalamide, N,N’-bis(2-hydroxyethyl)terephthalamide and terephthalic dihydrazide obtained through aminolytic depolymerization of polyethylene terephthalate waste. The data obtained has been analyzed to arrive at most appropriate values of essential parameters to obtain highly resolved HPLC chromatograms using odyssil C₁₈ column (4.6 × 250 mm, 5 μm) from Agela Technologies with a UV detector. Dimethyl formamide and dimethyl sulfoxide emerged as the most suitable mobile phases with an isocratic run of 10 min at a flow rate of 0.4 mL/minute. Effect of temperature and concentration on HPLC chromatograms was also investigated for N,N’-dibutylterephthalamide from 30 to 50 ℃ and 0.5 mg to 2.5 mg/10 mL of solvent, respectively. 1–2.5 mg/10 mL concentration was found to be most suitable with the column temperature of 40 ℃. Method validation consisted of linearity, intra- and inter-day precision, detection and quantitation limit. The validation experiments confirmed the precision of the present method, with RSD% and CV% values for both intra- and inter-day precision measuring below 1.9% and 0.5%, respectively. The method was linear in the range of 0.5–2.5 mg/10 mL solvent (R² = 0.98). Detection and quantitation limit were determined to be 1.32 and 4.02 mg/10 mL, respectively, for peak 1 and 0.90 and 2.75 mg/10 mL, respectively, for peak 2.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 4","pages":"215 - 226"},"PeriodicalIF":1.2,"publicationDate":"2024-02-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139924859","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":"Lipidomics Analysis of Different Marine Fish Oils Using Untargeted Liquid Chromatography–Orbitrap High-Resolution Mass Spectrometry and Chemometrics","authors":"Anjar Windarsih,&nbsp; Irnawati,&nbsp; Suratno,&nbsp;Hendy Dwi Warmiko,&nbsp;Lucky Prabowo Miftachul Alam,&nbsp;Indrawati Dian Utami,&nbsp;Abdul Rohman,&nbsp;Anastasia Wheni Indrianingsih","doi":"10.1007/s10337-024-04312-4","DOIUrl":"10.1007/s10337-024-04312-4","url":null,"abstract":"<div><p>Marine fish oils (MFOs) have been known for their nutritional compounds, which benefit human health. MFOs contain various lipids which play an essential role in human nutrition. The objective of this research was to apply untargeted lipidomics analysis using liquid chromatography–high-resolution mass spectrometry (LC–HRMS) for the comprehensive identification of lipid compositions extracted from five different marine fishes, namely red snapper (<i>Lutjanus campechanus</i> (A1))<i>,</i> giant grouper (<i>Epinephelus lanceolatus</i> (A2)), baronang crochet (<i>Siganus canaliculatus</i> (B2)), white snapper (<i>Lates calcarifer</i> (C3)), skipjack tuna (<i>Katsuwonus pelamis</i> (D2)). More than 1000 lipid compounds from both positive and negative ionization modes could be detected in each MFO using LC–HRMS untargeted lipidomics analysis. Most lipids were dominated by triglycerides (TG) and diglycerides (DG) classes. Principal component analysis (PCA) and partial least square-discriminant analysis (PLS-DA) could classify MFO samples in positive and negative ionization modes. Based on variable importance for projections (VIP) value, 15 differentiating lipid compounds were found to have an essential role as potential biomarkers in positive ionization mode. In contrast, ten differentiating lipid compounds were found in negative ionization mode. It can be concluded that untargeted lipidomics using LC–HRMS could be used as a powerful analytical technique for comprehensively identifying lipid compositions in MFO samples. It can be further used to identify the lipid compositions of other fish oil samples.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 4","pages":"203 - 214"},"PeriodicalIF":1.2,"publicationDate":"2024-02-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139750494","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":"Congress, Conferences, and Workshops","authors":"","doi":"10.1007/s10337-024-04317-z","DOIUrl":"10.1007/s10337-024-04317-z","url":null,"abstract":"","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 3","pages":"191 - 193"},"PeriodicalIF":1.2,"publicationDate":"2024-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142410542","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}