Journal of Chromatography A最新文献

{"title":"Modeling and techno-economic analysis of downstream manufacturing process intensification strategies for existing biopharmaceutical facilities","authors":"Juan J. Romero ,&nbsp;James Angelo ,&nbsp;Xuankuo Xu ,&nbsp;Scott M. Husson ,&nbsp;Sanchayita Ghose","doi":"10.1016/j.chroma.2024.465431","DOIUrl":"10.1016/j.chroma.2024.465431","url":null,"abstract":"<div><div>Downstream process (DSP) intensification technologies have the potential to provide faster, more sustainable, and more profitable processes. Nevertheless, the calculation of the possible benefits obtained from the implementation of these technologies is not always evident and usually depends on a particular production scenario. In the present work, we developed a framework for techno-economic feasibility analysis to assess the impact of changes in protein A capture, polishing, and viral filtration on process performance. The simulation used in this analysis is based on fundamental knowledge of the process and incorporates previously developed tools for calculating multi-column chromatography (MCC) and ultrafiltration-diafiltration variables. This framework was used to simulate production scenarios featuring intensified production schedules, increases in feed titers, MCC, integrated batch polishing, and high throughput viral filtration. These process alternatives were compared through key performance indicators that were selected to address specific questions on the suitability of these process intensification strategies in a particular context. Results were presented graphically for decision-makers to easily identify the best process alternatives for a given production scenario. For the conditions proposed in this work, we find that the scheduling practices, and not the unit operation processing times, have the greatest impact on process productivity. For instance, doubling the harvesting frequency resulted in a productivity increase of up to 61 %. Meanwhile, technological intensification strategies like MCC cause the greatest impact on operating costs, reducing cost of goods of the DSP by up to 27 %. Overall, intensification of individual unit operations can yield benefits from a sustainability and cost perspective, but to achieve higher throughputs, it is necessary to have fully intensified DSP and scheduling practices.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1737 ","pages":"Article 465431"},"PeriodicalIF":3.8,"publicationDate":"2024-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142492169","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of anthraquinones in Frangula alnus by Supercritical Fluid Chromatography","authors":"Michael Zwerger ,&nbsp;Anna Deisl,&nbsp;Fabian Hammerle,&nbsp;Markus Ganzera","doi":"10.1016/j.chroma.2024.465432","DOIUrl":"10.1016/j.chroma.2024.465432","url":null,"abstract":"<div><div>Anthraquinones are the major bioactive compounds in alder buckthorn<em>,</em> a plant with a long history of use for the treatment of obstipation in European and Asian traditional medicine. As these metabolites are also associated with toxic side effects, reliable analytical techniques for their determination are essential. Previously described methods mainly utilized Liquid Chromatography for this purpose, as the photometric assay described in the current edition of the European Pharmacopoeia lacks selectivity. In this study, the development and application of an alternative approach, Ultra-High Performance Supercritical Fluid Chromatography, is presented, facilitating the qualitative and quantitative determination of seven anthraquinone derivatives in under six minutes. This was possible by using a Torus™ DIOL column and a modifier comprising methanol with 10 % acetonitrile and 2.5 mM oxalic acid; applying a flow rate of 1.6 mL/min and an elevated temperature of 55 °C enabled optimal resolution. Regarding selectivity, linearity (R² ≥ 0.9995), precision and accuracy (recovery rates between 96.6 and 103.3 %), all results were in line with the respective ICH requirements. Practical applicability of the assay was confirmed by analyzing different samples, including commercially available plant material, phytopharmaceuticals containing <em>Frangula</em> bark and wild collected samples. Except of the latter, glucofrangulin A always was the dominating compound; however, the overall anthraquinone content showed to be very variable ranging from 2.18 to 51.32 mg.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1737 ","pages":"Article 465432"},"PeriodicalIF":3.8,"publicationDate":"2024-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142445703","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Rapid Determination of Trace Ethylene Glycol and Diethylene Glycol in Propylene Glycol-Contained Syrups by Ultrahigh-Performance Supercritical Fluid Chromatography-Mass Spectrometry after Precolumn Derivatization","authors":"Si-Tong Zheng ,&nbsp;Zi-Ying Wang ,&nbsp;Zhen Liu ,&nbsp;Yingxiang Du ,&nbsp;Ling Cao ,&nbsp;Sheng Tang ,&nbsp;Hian Kee Lee ,&nbsp;Yaozuo Yuan ,&nbsp;Hai-Wei Shi","doi":"10.1016/j.chroma.2024.465433","DOIUrl":"10.1016/j.chroma.2024.465433","url":null,"abstract":"<div><div>Ethylene glycol (EG) and diethylene glycol (DEG) are two contaminants known to cause a variety of human health problems, when ingested in certain amounts, they can cause adverse effects such as nephrotoxicity, neurotoxicity and even death. They are widely found in propylene glycol, which is commonly used as a base for pharmaceutical syrups. The aim of this study was to develop an analytical method for the evaluation of EG and DEG in commercially available pediatric syrups. In this study, a fast, simple and reliable ultrahigh performance supercritical fluid chromatography-electrospray ionization-mass spectrometry (UHPSFC-ESI-MS) method was developed. The work involved the evaluation of three derivatization reagents for UHPSFC-ESI-MS. Benzoyl chloride was finally selected as the optimal derivatization reagent. Compared with an approach without derivatization, the present method achieved the separation and detection of EG and DEG efficiently, sensitively and rapidly, and analysis of EG and DEG in syrup formulations was realized within 7 min. The linear determination coefficients of EG and DEG in the concentration range of 0.25–25.0 μg/mL were greater than 0.999. The limits of detection for EG and DEG were 0.02 μg/mL and 0.07 μg/mL, respectively, and the limits of quantification were 0.09 μg/mL and 0.25 μg/mL, respectively. The recovery rates of DEG and EG ranged from 85.5%–108.1% and 86.7%–117.2%, respectively. The absolute values of the matrix effects in the three types of syrups considered were all less than 10%. Meanwhile, a gas chromatography-hydrogen flame ionization detection method was established for cross-testing of the analytical results. In 10 batches of syrup formulations, DEG was not detected by either method. The presence of EG was detected by UHPSFC-ESI-MS in only three batches, none of which exceeded 90.23 parts per million (ppm), with a mean absolute error of 5.95 ppm between the two sets of results. The developed UHPSFC-ESI-MS method was rapid, simple, efficient, sensitive and accurate for the determination of EG and DEG in genuine syrup formulations.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1737 ","pages":"Article 465433"},"PeriodicalIF":3.8,"publicationDate":"2024-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142454799","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Analysis of interactions between pharmaceuticals and humic acid: Characterization using entrapment and high-performance affinity microcolumns","authors":"Sadia Sharmeen ,&nbsp;Isaac Kyei ,&nbsp;Arden Hatch ,&nbsp;Kyungah Suh ,&nbsp;Saumen Podder ,&nbsp;Sazia Iftekhar ,&nbsp;Daniel D. Snow ,&nbsp;David S. Hage","doi":"10.1016/j.chroma.2024.465427","DOIUrl":"10.1016/j.chroma.2024.465427","url":null,"abstract":"<div><div>The presence of pharmaceuticals as microcontaminants in the environment has become of particular concern given the growing increase in water reuse and recycling to promote global sustainability of this resource. Pharmaceuticals can often undergo reversible interactions with soluble dissolved organic material such as humic acid, which may be an important factor in determining the bioavailability and effects of these compounds in the environment. In this study, high-performance affinity microcolumns containing non-covalently entrapped and immobilized humic acid are used to examine the binding strength and interactions of this agent for tetracycline, carbamazepine, ciprofloxacin, and norfloxacin, all common pharmaceutical microcontaminants known to bind humic acid. The binding constants, as measured with Aldrich humic acid, have good agreement with values reported in the literature. In addition, the effects of temperature, ionic strength, and pH on these interactions are examined with the humic acid microcolumns. This technique makes it possible to determine the relative importance of electrostatic interactions vs non-polar interactions or hydrogen bonding on these binding processes. This study illustrates how affinity microcolumns can be used to screen and uniformly quantify binding by pharmaceuticals with humic acid, as well as to study the mechanisms of these interactions, with this information often being acquired in minutes and with small amounts of binding agent (∼10 mg per microcolumn, which could be used over 200–300 experiments). Use of entrapment and affinity microcolumns can support similar research for a wide range of other microcontaminants with humic acid or alternative binding agents found in water and the environment.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1737 ","pages":"Article 465427"},"PeriodicalIF":3.8,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142445707","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Highly selective split intein method for efficient separation and purification of recombinant therapeutic proteins from mammalian cell culture fluid","authors":"Sai Vivek Prabhala ,&nbsp;Brian Marshall ,&nbsp;Jackelyn Galiardi ,&nbsp;Yamin Fan ,&nbsp;Ekaterina Creamer ,&nbsp;David W. Wood","doi":"10.1016/j.chroma.2024.465430","DOIUrl":"10.1016/j.chroma.2024.465430","url":null,"abstract":"<div><div>Biologics and vaccines have been successfully developed over the last few decades to treat many diseases. Each of these drugs must be highly purified for clinical use. Monoclonal antibodies (mAbs), the dominant therapeutic modality on the market, can be easily purified using the standard Protein A affinity platform. However, no generally applicable affinity platforms are available for the manufacture of other therapeutic proteins for clinical use. Thus, multicolumn chromatography processes for widely being used for product purification. These processes demand significant optimization to meet desired product quality attributes, where each step also decreases final yields. In this work, we demonstrate the novel self-removing <em>i</em>CapTag™ affinity tag, which provides a new platform for capturing, concentrating, and purifying recombinant proteins. Importantly, this system provides a tagless target protein, which is suitable for research and clinical use, where the only requirement for tag removal is a small change in buffer pH. No additional proteins, reagents or cofactors are required. We also present case studies demonstrating the use of <em>i</em>CapTag™ for highly efficient purification of untagged interferon alpha 2b, the ML39 single chain variable fragment (scFv), and the receptor binding domain (RBD) of SARS-CoV-2 spike protein. These proteins were expressed and secreted by Expi293 cells with the self-removing tag fused to their N-terminus. We were able to obtain highly pure (&gt; 99 %) tagless protein in a single purification step with high clearance of host cell DNA, tagged precursor, higher and lower molecular weight impurities. Based on these preliminary results, we propose the <em>i</em>CapTag™ as a universal capture platform for diverse classes of recombinant therapeutic proteins.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1736 ","pages":"Article 465430"},"PeriodicalIF":3.8,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142433442","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Comparison of experimental and simulated separation performance in capillary tube-in-manifold devices","authors":"Christopher Piccolo ,&nbsp;Michael Keller ,&nbsp;Daniel J. Czarnecki ,&nbsp;Thomas Austin ,&nbsp;Graham Shelver ,&nbsp;James P. Grinias","doi":"10.1016/j.chroma.2024.465428","DOIUrl":"10.1016/j.chroma.2024.465428","url":null,"abstract":"<div><div>A metal tube-in-manifold packed bed capillary column device, designed to overcome common limitations associated with capillary LC separations, is described. Experimental results of initial packing tests with sub-3 μm core-shell particles demonstrated efficiencies greater than 47,000 plates/m for a separation performed using the column device. Computational fluid dynamics (CFD) modeling of the multicomponent separation used for this work was validated against experimental LC results and the optimized model was able to effectively predict component peak retention times. However, the accuracy of predicted efficiencies requires further refinement. The tube-in-manifold design demonstrates that packed capillary columns with cylindrical cross-sectional channel geometry and ultrahigh pressure, low dead volume fluidic connections are achievable.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1736 ","pages":"Article 465428"},"PeriodicalIF":3.8,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142434010","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Wide-pore fully porous mixed-mode octyl/pyridyl-bonded silica material with pH-dependent surface charge reversal for high-performance hydrophobic charge-induction chromatography of proteins","authors":"Marc Wolter ,&nbsp;Christoph Barth ,&nbsp;Mirna Maalouf ,&nbsp;Markus Kramer ,&nbsp;Adrian Sievers-Engler ,&nbsp;Michael Lämmerhofer","doi":"10.1016/j.chroma.2024.465429","DOIUrl":"10.1016/j.chroma.2024.465429","url":null,"abstract":"<div><div>In an attempt to overcome silanophilic interactions like observed on popular reversed-phase butyl‑bonded silica stationary phases in protein HPLC, a mixed-mode stationary phase based on wide pore silica (3 µm, 300 Å) was prepared by co-immobilization of octyl and 2-pyridylethyl ligands. The surface modification was performed by a new approach using synthesized functional silatranes of the above ligands and prewetted silica. It allowed to generate a dense polymeric siloxane layer on the silica surface. Butyl-bonded silica and octyl/3-aminopropyl-bonded mixed-mode silica phases were prepared for comparison. The modified silicas were subsequently characterized by elemental analysis regarding ligand densities, by solid-state ²⁹Si and ¹³C cross polarization/magic angle spinning nuclear magnetic resonance spectroscopy for confirming the surface-bonded structure, and by pH-dependent ζ-potential measurements via electrophoretic light scattering providing net surface charge information at distinct pH values. While the classical butyl‑bonded stationary phase revealed negative ζ-potential over the entire pH range investigated (pH 3.5–9.5) due to residual silanols and the mixed-mode octyl/3-aminopropyl-bonded silica positive ζ-potential over the entire pH range, pH-dependent charge reversal was observed at approximately pH 5.5 for the octyl/pyridyl-bonded stationary phase. Then, a test set of proteins differing in hydrophobicities and isoelectric points was employed to evaluate the retention characteristics of all three synthesized stationary phases over the pH range of 3 to 7.5 by acetonitrile-gradient elution reversed-phase HPLC. Under acidic conditions (pH 3) the mixed-mode phases octyl/pyridyl-silica and octyl/aminopropyl-silica showed reduced retention and improved peak shapes due to repulsive interactions preventing silanophilic interactions, while protein separations by their hydrophobicities were achieved (repulsive charge-assisted protein RPLC). Finally, the prepared novel mixed-mode octyl/pyridyl-bonded stationary phase was evaluated in hydrophobic charge induction chromatography mode for protein separation of the same test set. Instead of an organic modifier gradient, elution was enforced by a pH gradient from almost neutral to acidic pH at constant organic modifier content of 10 %. This chromatographic mode showed orthogonal retention characteristics and reversed elution order compared to above organic gradient RP-HPLC. In addition, significantly less organic solvent was used under these conditions, classifying it as a green protein LC technology.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1737 ","pages":"Article 465429"},"PeriodicalIF":3.8,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142454800","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A charge reversal approach for the sensitive quantification of dicarboxylic acids using Liquid chromatography-tandem mass spectrometry","authors":"Joby Jose,&nbsp;Alfred N Fonteh","doi":"10.1016/j.chroma.2024.465426","DOIUrl":"10.1016/j.chroma.2024.465426","url":null,"abstract":"<div><div>Dicarboxylic acids (DCAs) are essential for intermediate metabolism and are implicated in multiple processes associated with various diseases. Several DCAs contribute to energy metabolism, impact mitochondrial function, and play a crucial role in body function. However, the low abundance of some DCAs in various body fluids makes their quantification particularly challenging. Therefore, an extremely sensitive method is required to determine DCA level fluctuations in biological samples in different diseases. We developed and optimized an LC-MS/MS method to quantify DCAs. We achieved charge reversal of the compounds from negative to positive ionization through chemical derivatization with dimethylaminophenacyl bromide (DmPABr) targeting the carboxyl group (R-COOH) under mild basic conditions. Derivatization enhanced sensitivity, mass fragmentation, and chromatographic separation for LC-tandem mass spectrometric quantification. The method was analytically optimized and demonstrated excellent linearity for individual DCAs (R²&gt;0.99), as well as an exceptionally lower limit of detection (LLOD&lt;266 fg) and lower limit of quantification (LLOQ&lt;805 fg) for all DCAs. Furthermore, most derivatized DCAs were stable at room temperature and after ten repeated freeze−thaw cycles. After DCA extraction and quantification detection, we found differences in their distribution in plasma and urine. The rank order for DCAs in plasma is C4&gt;C6&gt;C7&gt;C9&gt;C5&gt;C8&gt;C22, whereas in the urine sample, the order is C4&gt;C7&gt;C6&gt;C9&gt;C5&gt;C8&gt;C10. For longer chains (C &gt; 16), their proportions were &gt;10x higher in plasma than in urine. Our optimized method using LC-MS/MS enables the quantification of DCAs with excellent sensitivity. The method will help in future studies investigating dicarboxylic acids' crucial role in health and biomarker discovery studies using targeted metabolomics.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1737 ","pages":"Article 465426"},"PeriodicalIF":3.8,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142445706","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Transgender Women with HIV Demonstrate Unique Non-Alcoholic Fatty Liver Disease Profiles.","authors":"Jordan E Lake, Ana N Hyatt, Han Feng, Hongyu Miao, Anoma Somasunderam, Netanya S Utay, Kathleen E Corey","doi":"10.1089/trgh.2022.0182","DOIUrl":"10.1089/trgh.2022.0182","url":null,"abstract":"<p><strong>Purpose: </strong>Non-alcoholic fatty liver disease (NAFLD) prevalence and severity may be higher in people with human immunodeficiency virus (HIV) than the general population, and vary with sex and age. We explored NAFLD characteristics by gender.</p><p><strong>Methods: </strong>Adult transgender women (TW), cisgender women (CW), and cisgender men (CM) with HIV on antiretroviral therapy and without other known causes of liver disease underwent screening for NAFLD (2017-2020). Circulating factors associated with NAFLD were measured. Hepatic steatosis and fibrosis were assessed using transient elastography by controlled attenuation parameter (CAP) and liver stiffness measurement (LSM), respectively. Analysis of variance/Wilcoxon testing compared normally/non-normally distributed variables, respectively. Logistic regression evaluated factors associated with CAP and LSM.</p><p><strong>Results: </strong>Participants (<i>n</i>=194) had median age 48 years and body mass index 28.3 kg/m²; 42% were CM, 37% TW, and 21% CW; 95% were non-white; and 16% had diabetes, 40% dyslipidemia, and 49% hypertension. NAFLD prevalence was 59% using CAP ≥248 dB/m (≥S1 steatosis), 48% using CAP ≥260 dB/m (≥S2 steatosis), and 32% using CAP ≥285 dB/m (≥S3 steatosis). Compared to CM and CW, TW had the highest median CAP scores, were more likely to have ≥S2 steatosis, and had the highest insulin resistance, interleukin-6, and fetuin-A values. TW off versus on gender-affirming hormone therapy (GAHT) had slightly higher median CAP scores.</p><p><strong>Conclusion: </strong>TW on GAHT had less hepatic steatosis than TW not on GAHT, although overall NAFLD severity was greater than expected for TW compared to CM and CW. The effects of estrogen supplementation and androgen deprivation on liver health in TW require further study.</p>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1632 ","pages":"413-420"},"PeriodicalIF":2.0,"publicationDate":"2024-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11496901/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41279292","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Macrocyclic anti-inflammatory diterpenes from the South China Sea soft coral Sinularia erecta and their isolation by combined column chromatography","authors":"Song-Wei Li ,&nbsp;Cristina Cuadrado ,&nbsp;Jiao Liu ,&nbsp;Heng Li ,&nbsp;Wei Tang ,&nbsp;Antonio Hernandez Daranas ,&nbsp;Yue-Wei Guo","doi":"10.1016/j.chroma.2024.465416","DOIUrl":"10.1016/j.chroma.2024.465416","url":null,"abstract":"<div><div>Eleven new macrocyclic casbane-type diterpenes, namely sinueracasbanones E–O (<strong>1</strong>–<strong>11</strong>), have been isolated from the South China Sea soft coral <em>Sinularia erecta</em> using combined column chromatography. The structures of new compounds were elucidated by extensive spectroscopic data analysis, the modified Mosher's method, X-ray diffraction analysis and quantum mechanical calculation methods. In bioassay, compounds <strong>2, 5, 10</strong> and <strong>11</strong> displayed interesting anti-inflammatory activities by the inhibition of lipopolysaccharide (LPS)-induced tumor necrosis factor (TNF)-α protein release with half maximal inhibitory concentration (IC₅₀) values of 15.6, 7.1, 13.7 and 6.6 µM, respectively.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1736 ","pages":"Article 465416"},"PeriodicalIF":3.8,"publicationDate":"2024-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142426335","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}