Chromatographia最新文献

{"title":"New Comb-Like Polyelectrolytes in Capillary Electrophoresis","authors":"Aleksandra A. Adamova,&nbsp;Mikhail S. Orlov,&nbsp;Nadezhda S. Rakovskaya,&nbsp;Petr A. Fetin,&nbsp;Lyudmila A. Kartsova","doi":"10.1007/s10337-024-04376-2","DOIUrl":"10.1007/s10337-024-04376-2","url":null,"abstract":"<div><p>New comb-like polyelectrolytes with triethylammonium (pAUTEA-Br), N-methyl-piperidinium (pAUMP-Br), N-methyl-morpholinium (pAUMM-Br) and pyridinium (pAUPy-Br) cation groups were first used to separate steroid hormones, biogenic amines and amino acids under capillary electrophoresis conditions. The polymers acted as modifiers of electrophoretic systems and were used as dynamic coatings of inner surface of fused-silica capillary and additives to background electrolyte to perform capillary electrochromatography and micellar electrokinetic chromatography regimes, leading to increase in separation selectivity and efficiency, and as reagents for indirect spectrophotometric detection of amino acids. New materials also showed activity during on-line preconcentration of biogenic amines and reduced their limits of detections by 10 times. Thus, new comb-like polyelectrolytes were demonstrated to act as multifunctional materials for capillary electrophoresis. This study discusses the features of the influence of the polyelectrolytes on electrophoretic separation capabilities and their possibilities in separation of model biologically active substances. Modifiers of this type significantly expand the analytical capabilities of the capillary electrophoresis method.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 1","pages":"33 - 43"},"PeriodicalIF":1.2,"publicationDate":"2024-11-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143110174","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 and Structural Characterization of New Degradation Products in Moxidectin Stressed Samples by LC-HRMS and NMR","authors":"Jingzhi Tian,&nbsp;Abu M. Rustum,&nbsp;Sarju Adhikari","doi":"10.1007/s10337-024-04375-3","DOIUrl":"10.1007/s10337-024-04375-3","url":null,"abstract":"<div><p>Moxidectin (MOX) is a macrocyclic lactone which belongs to milbemycin family of antiparasitic endectocides. MOX is widely used in veterinary medicine for the treatment and control of external and internal parasites, MOX is also used for the treatment of onchocerciasis (river blindness) in humans. In this paper, MOX drug substance was subjected to acidic, alkaline, oxidation, thermal (solid and solution state), and photolytic (solid and solution state) stress degradation. Stress-degraded samples of MOX were analyzed by a reversed phase ultra performance liquid chromatography (RP-UPLC) method using HALO C18 column (100 × 2.1 mm, 2 µm). MOX and all major DPs were adequately separated by a gradient elution using 0.1% formic acid in water as mobile phase-A and acetonitrile as mobile phase-B. Total 12 major DPs, including seven new DPs (2-carboxyl-19-hydroxyl, 2-carboxyl-3,4-epoxy-19-hydroxyl, 14,15-epoxide, 26,27-epoxide, 14-OOH, 15-OOH, and 27-OOH) not previously reported in the literature, were observed. Structural characterization of these DPs was performed using UPLC-high resolution mass spectrometry (HRMS) and by comparison of their fragmentation profile with parent compound. Six major DPs namely 3,4-epoxide, 14,15-epoxide, 26,27-epoxide, 14-OOH, 15-OOH, and 27-OOH were isolated and purified from the stressed samples using semi-preparative HPLC. The chemical structures of these DPs were further confirmed through comprehensive nuclear magnetic resonance (NMR) spectroscopy studies. The study results reported in this paper should be helpful to further understand degradation pathways of MOX under different conditions. These results are also beneficial to facilitate quality monitoring of MOX drug substance as well as identification of unknown degradation products in drug formulations made with MOX drug substance.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 1","pages":"57 - 69"},"PeriodicalIF":1.2,"publicationDate":"2024-11-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143108778","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":"Systematic Development of a Gradient Elution HPLC Method for the Analysis of Voxelotor and Its Structurally Related Substances Applying Analytical Quality by Design Approach","authors":"Siva Ganesh Bommi,&nbsp;Subbalakshmi Jayanty,&nbsp;Suresh Kola,&nbsp;Venkata Siva Rama Krishna Reddy Kallam","doi":"10.1007/s10337-024-04378-0","DOIUrl":"10.1007/s10337-024-04378-0","url":null,"abstract":"<div><p>Sickle cell disease is a genetic disorder treated with Voxelotor (Vox), the first hemoglobin oxygen-affinity regulator. Although Vox recently received expedited approval in the United States for the sickle cell disease therapy for certain age groups, no monograph is yet available in the official compendia for Vox. Therefore, current study aims to develop a stability-indicating HPLC method for determining five potential impurities in Vox drug substance. The procedure was developed by implementing principles of analytical quality by design (AQbD). A detailed risk evaluation was conducted in accordance with the cause-and-effect relationship. A factorial design was employed to identify the impact of the critical method parameters (CMPs) and their relationship to critical quality attributes (CQAs). The full factorial design was utilized and final method was optimized. The <i>p</i>-values of the model and lack of fit were &lt; 0.0001 and &gt; 0.05, respectively, indicating the best-fit statistical model for the studied responses. The CMPs, such as gradient slope (ratio of mobile phase-B % and gradient time), flow rate of 1.0 mL min⁻¹, and column oven temperature of 40 °C, were optimized from the full factorial design. The best possible separation among all impurities and Vox was achieved with gradient elution using X-Bridge C₁₈, 150 mm × 4.6 mm, 3.5 µm analytical column. The optimized gradient is time (min)/%B: 0.0/15, 3.0/15, 20.0/80, 30/80, 31/15, 35/15. The peak pairs where the separation was highly critical were: impurity-4/impurity-5 and impurity-5/Vox. Method validation, revealed that the mean recovery of the impurities ranged between 100 and 106%, the correlation coefficient (<i>r</i>) &gt; 0.99, across the span for LOQ–150% levels, RSD values (<i>n</i> = 6) ranged between 1.2 and 4.6% for 100% level (i.e., 0.1% of impurities). The peaks from the specificity analysis did not intervene with the known and active analyte (Vox) peak and this study identified impurity-2 as a major degradation product.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 1","pages":"19 - 31"},"PeriodicalIF":1.2,"publicationDate":"2024-11-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143108877","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":"An UPLC Method for Determination of Structural Analogues of DM1: the Payload of Trastuzumab Emtansine (T-DM1)","authors":"Junliang Yao,&nbsp;Yang Zhu,&nbsp;Daquan Yin","doi":"10.1007/s10337-024-04377-1","DOIUrl":"10.1007/s10337-024-04377-1","url":null,"abstract":"<div><p>DM1, a derivative of maytansine, is the payload of trastuzumab emtansine (T-DM1). In this work, a new gradient reverse-phase ultra-performance chromatographic (RP-UPLC) method was proposed for analysis of five structural analogues (DM1-2, AP-3, DM1-4D, DM1-3D, and DM1-3L) of DM1. The chromatographic separation was accomplished by using a Waters BEH Phenyl column (50 × 2.1 mm, 1.7 μm), at the wavelength of 252 nm. Validation of the method was carried out according the ICH guidelines in terms of specificity, accuracy, precision, linearity and robustness. The developed method was proved to be convenient and reliable for quantitative determination of the DM1 analogue impurities. It can also be used for the related substances determination in DM1 bulk samples.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 1","pages":"11 - 18"},"PeriodicalIF":1.2,"publicationDate":"2024-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-024-04377-1.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143108730","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}

{"title":"Simultaneous Enrichment and Purification of Licorice Chalcone A and Isoliquiritigenin in Licorice Using a Mixed-Mode Monolith","authors":"Yijie Liu,&nbsp;Dan Zhang,&nbsp;Ligai Bai,&nbsp;Hongyuan Yan,&nbsp;Haiyan Liu","doi":"10.1007/s10337-024-04374-4","DOIUrl":"10.1007/s10337-024-04374-4","url":null,"abstract":"<div><p>In this paper, a mixed-mode monolith was prepared by separately synthesizing hydrophilic and hydrophobic materials at both ends of a chromatography column by a one-step method. The prepared mixed mode monolith was used as solid phase extraction adsorbent for simultaneous enrichment and purification of licorice chalcone A and isoliquiritigenin from licorice combined with high performance liquid chromatography (HPLC). It had superior ability to enrich and purify licorice chalcone A and isoliquiritigenin than single hydrophilic or hydrophobic monolith. The method had good linearity in the range of 0.50–400 μg/mL. The linear regression equation was y = 465.45 ×  − 1.04 and the correlation coefficient was 0.9999. The relative standard deviations (RSDs) of intra-day and inter-day precision were both less than 1.19%. The results showed that the method was simple and accurate, and could be used for the enrichment and purification of licorice chalcone A and isoliquiritigenin from licorice.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 1","pages":"45 - 55"},"PeriodicalIF":1.2,"publicationDate":"2024-10-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143110050","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":"Electrostatic Assembly of Graphene@SiO2 Composite for Enhanced Dispersive Solid-Phase Extraction: Targeting Eight Pesticide Residues","authors":"Sheng Liu,&nbsp;Bo Li,&nbsp;Jian Xu,&nbsp;Yang Yu,&nbsp;He Zhu,&nbsp;Zhen Li,&nbsp;Zhaoxue Zhang,&nbsp;Mei Lv,&nbsp;Litao Wang","doi":"10.1007/s10337-024-04372-6","DOIUrl":"10.1007/s10337-024-04372-6","url":null,"abstract":"<div><p>As a new carbon nanomaterial, graphene (Gr) has attracted wide attention in the field of separation and analysis because of its large specific surface area and strong hydrophobicity. A highly efficient and selective graphene/SiO₂ (Gr/SiO₂) dispersive solid-phase extraction (d-SPE) material was prepared through electrostatic assembly. This process involved the combination of negatively charged poly (sodium 4-styrenesulfonate) (PSS) mediated GS (denoted as PSS-GS) and positively-charged SiO₂, modified with triethoxy silane amino. The precursor material was characterized using FESEM, FTIR and so on. We evaluated the extraction performance of this new sorbent with eight pesticide residues, using the HPLC–MS method. The sorbent demonstrated excellent recovery rates for the pesticide residues under various frequency of use conditions and pH levels. It showed that the SiO₂ and Gr have synergistic extraction effect, and the composite material has good stability and reusable, Ultimately, this newly developed d-SPE material was successfully applied in the analysis of fruit juice samples, yielding good recovery rates in the range of 82.18 to 117.49%.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 1","pages":"1 - 9"},"PeriodicalIF":1.2,"publicationDate":"2024-10-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143109120","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":"Metabolites Identification of Two Novel Chemical Constituents From Melia. Toosendan Sieb.et Zucc. in Rats by UPLC/ESI/qTOF-MS Analysis","authors":"Yuan Liu,&nbsp;Ranchen Xu,&nbsp;Siqi Gu,&nbsp;Shuning Li,&nbsp;Ye Fang,&nbsp;Anam Naseem,&nbsp;Yan Liu,&nbsp;Bingyou Yang","doi":"10.1007/s10337-024-04373-5","DOIUrl":"10.1007/s10337-024-04373-5","url":null,"abstract":"<div><p><i>Melia. toosendan</i> Sieb.et Zucc., a potent herbal medicine, boasts diverse therapeutic properties. As the main components, the isotoosendanin blocks protective autophagy in chemotherapy-induced cultured cancer cells and xenograft tumor tissue to significantly enhancing anticancer activity, and the fraxinellone contributes to pesticidal activity, anti-inflammatory and immunomodulatory effects. Until now, the metabolic profiles remained unknown. In the present study, 13 metabolites of isotoosendanin and 13 metabolites of fraxinellone were characterized in the blood, urine, and feces of rats by UPLC/ESI/qTOF-MS analysis. Five metabolites (F-M3, F-M5, I-M1, I-M5, I-M8) were fully characterized. The isotoosendanin and fraxinellone were mainly involved in hydrogenation, acetylation, and methylenation metabolic reactions. This is the first study illuminates the two components in vivo metabolism, laying the foundation for future pharmacodynamic and mechanistic investigations. It is necessary to deeply understand the process of drug activation, and deactivation, rationally design new drugs, and guide the research and development of new drugs.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 1","pages":"71 - 80"},"PeriodicalIF":1.2,"publicationDate":"2024-10-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143108851","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":"Preparation of Restricted Access Media-Methacrylic Resin and Its Application as the Sorbent of Solid-Phase Extraction in the Lamotrigine Determination in Human Plasma by HPLC–UV","authors":"Xiaofei Wang,&nbsp;Qian Peng,&nbsp;Yumei Dong,&nbsp;Xiping Dou,&nbsp;Ping Li,&nbsp;Yinliang Bai","doi":"10.1007/s10337-024-04370-8","DOIUrl":"10.1007/s10337-024-04370-8","url":null,"abstract":"<div><p>Restricted Access Media-Methacrylic Resin with the ability of protein exclusion was prepared by the free radical polymerization using methacrylic acid, ethylene glycol dimethacrylate and glycidyl methacrylate as monomer, cross-linker and comonomer, respectively. Protein exclusion ability of this material was studied. The results showed that the material was able to eliminate 93.6% of protein after bovine serum albumin solution was added and shaken for 220 min. Adsorption kinetics and adsorption isotherms of Lamotrigine on this material were investigated. The experimental data were the most suitable for the pseudo-second-order kinetics model and Freundlich isotherm model. Restricted Access Media-Methacrylic Resin was used as sorbent for Solid-Phase Extraction to extract Lamotrigine from Human Plasma. The method for the determination of Lamotrigine in human plasma by SPE followed by the HPLC–UV presented linear range from 1.0 to 66.6 µg/mL with correlation coefficient 0.9930 for Lamotrigine, assay precision with relative standard deviation value 6.24%, and assay accuracy 94.7–104.7% with relative standard deviation values 4.33–5.81%. SPEs filled with this material were used at least 7 times without any significant changes in their performance. Analytical validation parameters demonstrated that the method could be applied to the determination of Lamotrigine at the therapeutic plasma levels without other treatments.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 11-12","pages":"729 - 737"},"PeriodicalIF":1.2,"publicationDate":"2024-10-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142694779","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":"Shortening the Analysis Time of a “Ready-To-Use” Relative Response Factor Database-Coupled Pyrolyzer/Thermal Desorption–Gas Chromatography–Mass Spectrometry Method of Screening for Phthalate Esters, Polybrominated Diphenyl Ethers, and Polybrominated Biphenyls in Polymers","authors":"Yukihiko Kudo,&nbsp;Tomohiro Uchimura","doi":"10.1007/s10337-024-04371-7","DOIUrl":"10.1007/s10337-024-04371-7","url":null,"abstract":"<div><p>The European Union RoHS Directive restricts the presence of phthalate esters, polybrominated diphenyl ethers (PBDEs), and polybrominated biphenyls (PBBs) in electrotechnical products. The international standard IEC 62321-3-3 describes a method of screening for these chemicals using gas chromatography–mass spectrometry with a pyrolyzer/thermal desorption accessory (Py/TD-GC/MS). Although the IEC 62321-3-3 method is effective at determining levels of these restricted compounds in polymers, applying this method in RoHS testing poses two issues: it requires the preparation of a relative response factor (RRF) database from expensive standard mixed solutions, and it has a long analysis time (30 min). In a previous report, we described a method based on a “ready-to-use” RRF database that eliminates preparation of the RRF database. In this report, we resolved the remaining issue by improving the analytical throughput of the IEC 62321-3-3 method. By optimizing the Py/TD and GC/MS conditions, we almost halved the analysis time to 16 min while maintaining analytical accuracy. These optimized conditions were then combined with the above-mentioned “ready-to-use” RRF database to create a new method that resolves both of the issues with the IEC 62321-3-3 method. This new method demonstrated good sensitivity with a lower limit of detection of under 30 mg/kg for each target compound. We also assessed the analytical accuracy of this new method by analyzing various standard polymer materials on two different analytical instruments. On both instruments, the mean recovery rate was within 100 ± 30% for seven phthalate esters and for combined concentrations of PBDE and PBB congeners, which demonstrated that the quantitative accuracy of the new method is sufficient for RoHS testing. The new method resolves the issues with the IEC 62321-3-3 method and offers rapid, simple, and reliable screening that can be adopted for RoHS testing.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"88 1","pages":"81 - 92"},"PeriodicalIF":1.2,"publicationDate":"2024-10-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-024-04371-7.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143107824","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}

{"title":"Certification and Long-Term Stability Assessments of 5-Methyltetrahydrofolate in Spinach and Kimchi Cabbage Certified Reference Materials Using Tri-enzyme Method and Isotope Dilution Ultra-performance Liquid Chromatography/Tandem Mass Spectrometry","authors":"Seok-Won Hyung,&nbsp;Joonhee Lee","doi":"10.1007/s10337-024-04369-1","DOIUrl":"10.1007/s10337-024-04369-1","url":null,"abstract":"<div><p>This study presents the certification of spinach and kimchi cabbage certified reference materials (CRMs), (KRISS CRM 108-05-010 and 108-05-011), for 5-Me-THF. The fresh spinach and kimchi cabbage process involved washing, freeze-drying, pulverizing, sieving, V-mixing, and bottling in 10-g portions. The 5-Me-THF in the CRMs was then extracted and analyzed using a tri-enzyme method and isotope dilution ultra-performance liquid chromatography/tandem mass spectrometry. The method validation demonstrated that the method was both repeatable and reproducible, with the recovery ranging from 96.5 to 107.2%. The stability monitoring was performed for 7 days at room temperature, 1 month at − 20 °C, and 13 months at − 70 °C, confirming the stability of the CRMs under most conditions. The certified values were (16.93 ± 0.73) mg/kg and (11.66 ± 0.25) mg/kg for spinach and kimchi cabbage CRMs, respectively. The homogeneity of the CRMs was 1.85% and 0.91% for spinach and cabbage CRMs, respectively. Additional long-term stability assessments were performed, and this suggested that the CRMs will remain valid for at least another 48 months at − 70 °C.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"87 11-12","pages":"785 - 794"},"PeriodicalIF":1.2,"publicationDate":"2024-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142694763","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}