Journal of Chromatography A最新文献

{"title":"A charge reversal approach for the sensitive quantification of dicarboxylic acids using Liquid chromatography-tandem mass spectrometry","authors":"","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":null,"pages":null},"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":"Macrocyclic anti-inflammatory diterpenes from the South China Sea soft coral Sinularia erecta and their isolation by combined column chromatography","authors":"","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":null,"pages":null},"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}

{"title":"A comprehensive review of portable syringe systems using micropipette-based extraction techniques for metal analysis","authors":"","doi":"10.1016/j.chroma.2024.465423","DOIUrl":"10.1016/j.chroma.2024.465423","url":null,"abstract":"<div><div>The release of harmful compounds, particularly dangerous metal ions, into the environment has drawn deep concern from the scientific community. Therefore, it has become common in research to evaluate and quantify the harmful concentrations in the presence of these metal ions in several real samples (food, water, and biological samples). To increase sensitivity and lessen the impact of the matrix, sample pretreatment is a helpful strategy to implement before analysis. The limitations of conventional methods have been recently significantly reduced by developing new analytical approaches such as microextraction techniques. The miniaturization of conventional solid-phase extraction (SPE) led to solid-phase microextraction (SPME), drastically reducing both adsorbent use and extraction phase volume. SPME is defined in the present context as a modified extraction technique that employs a portable syringe system attached to micropipette tips. The SPME is considered one of the most appropriate sample preparation tools due to its compatibility with different detection techniques for different metal ions. The current review focuses on SPME based on a portable syringe (attaches to a micropipette tip) system because it has many advantages over conventional solid-phase extraction. It can be designed very simply in a syringe system, a very small quantity of the sorbent has to be kept in the tip, tube, or inside a syringe as a plug and combined with various analytical instruments. Many researchers have designed their own by using homemade tips packed with a sorbent to increase extraction capability and selectivity. According to the current review, there is a lot of potential for increasing the efficacy and efficiency of metal ion extraction from complicated matrices using portable syringe SPME. Studies have shown that when compared to conventional approaches, it performs better in terms of sensitivity, selectivity, and user-friendliness. Furthermore, its application to a wider range of sample types has been enhanced by the flexibility in constructing unique sorbent tips. Conclusively, the developments in portable syringe SPME have addressed several limitations of conventional techniques, positioning it as a robust and versatile tool for environmental monitoring and analysis of hazardous metal ions.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-10-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142446045","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":"Comprehensive characterization of active components in Salvia miltiorrhiza using polarity-partitioned two-dimensional liquid chromatography coupled with mass spectrometry","authors":"","doi":"10.1016/j.chroma.2024.465424","DOIUrl":"10.1016/j.chroma.2024.465424","url":null,"abstract":"<div><div><em>Salvia miltiorrhiza</em>, a widely used traditional Chinese medicine, contains a complex matrix of hydrophobic diterpenoids and hydrophilic phenolic acids, presenting significant challenges in comprehensive analysis. In this study, an online polarity-partitioned two-dimensional liquid chromatography coupled with mass spectrometry (2D-LC-MS) method was developed for comprehensive analysis of both lipophilic and hydrophilic active components in <em>Salvia miltiorrhiza</em>. The method integrated hydrophilic interaction liquid chromatography (HILIC) and reversed-phase liquid chromatography (RPLC), facilitating the efficient separation of compounds across a wide range of polarities. An online dilution strategy was implemented, minimizing sample loss and enhancing the method's utility for quality control and chemical characterization of complex herbal matrices. Compared with other LC methods, this approach significantly improved analyte coverage, resolution, and analysis efficiency. Under optimal conditions, 150 active components were successfully identified, including 33 compounds newly discovered in <em>Salvia miltiorrhiza</em>. Additionally, the validated online method was applied to the quantitative determination of 16 quality markers of <em>Salvia miltiorrhiza</em> from different sources. The results demonstrated the online method's potential as a superior alternative to existing techniques, offering broader applicability in traditional Chinese medicine research.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-10-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142434011","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":"Fabrication of sodium alginate doped phosphoric acid composite hydrogel and its application of the adsorption of La (III) in wastewater","authors":"","doi":"10.1016/j.chroma.2024.465425","DOIUrl":"10.1016/j.chroma.2024.465425","url":null,"abstract":"<div><div>Recycling rare earth ions from wastewater is an important task, as rare earth elements have a wide range of applications and can cause harm to the environment if discharged arbitrarily. In this work, a simple and inexpensive hydroxyethylidene diphosphate-based adsorbent (SA@HEDP) for adsorbing lanthanum was designed and fabricated. The adsorbent SA@HEDP with the surface rich in phosphate and hydroxyl functional groups provided active sites for adsorption of lanthanum. Research on adsorption performance was conducted by testing the amount of HEDP added, the amount of adsorbent used, the effect of initial pH of La (III), adsorption time, and temperature. The results showed that the adsorption capacity of the adsorbent was 158.0 mg/g. Adsorption of La (III) in real wastewater was tested, when the initial concentration of La (III) was 319.2 mg/L, it could be basically all recovered through three adsorption processes. SEM, EDS mapping, XPS, FTIR, and Zeta potential were used to characterize and analyze the mechanism, and mass transfer kinetics was used to analyze the adsorption process of the adsorbent for La (III).</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-10-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142405822","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":"Separation of polyphenols by HILIC methods with diode array detection, charged aerosol detection and mass spectrometry: Application to grapevine extracts rich in stilbenoids","authors":"","doi":"10.1016/j.chroma.2024.465422","DOIUrl":"10.1016/j.chroma.2024.465422","url":null,"abstract":"<div><div>The characterization of plant extracts is usually accomplished by reverse-phase liquid chromatography, but the development of new complementary approaches, such as HILIC, offers an orthogonal method. In this study, five HILIC stationary phases were evaluated to assess their ability to retain polyphenols. They were selected to cover the main different HILIC mechanisms: bare silica; silica with ethylene bridge; neutral amide; amino; zwitterionic. A total of 31 polyphenol standards were used for the screening, including 9 stilbenes, 8 flavonoids, 6 anthocyanins, and 8 phenolic acids. Three different detections were tested: diode array detector, charged aerosol detector and mass spectrometry.</div><div>Results indicated that silica supports were not suitable for retaining polyphenols, with no or low retention observed except for anthocyanins. The effectiveness of stationary phases in retention of phenolics following the order related to increased retention: zwitterionic, amide, and amino.</div><div>The choice of mobile phase also influenced retention. Mobile phases containing TFA as pH modifier limited retention, while formic acid was found to be more effective for polyphenol retention. Ammonium buffers also improved retention but often compromised peak shape. pH changes mainly impacted ionizable compounds, such as phenolic acids, by increasing their retention when they were ionized.</div><div>DAD was wellsuited for detecting polyphenols that possess aromatic rings, though peak wavelengths depend on the structures of the polyphenols. CAD, while less sensitive than DAD and MS, provided an almost similar response for structurally related compounds, even with gradient elution. MS was the preferred detector for quantification when resolution between compounds was challenging, as it is often the case with natural extracts.</div><div>The study successfully demonstrated that best HILIC conditions were obtained using an amino stationary phase composed of a polyethylenimine and formic acid-based mobile phase. These conditions were successfully applied to the analysis of stilbenoid-rich extracts from different parts of the vine. The elution order of stilbenoids followed the degree of polymerization. With CAD, the chromatographic profile was more representative of sample composition. It was demonstrated for the first time the interest of a combination of HILIC and CAD for analyzing stilbenes, offering a complementary approach to the classic RP analysis.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-10-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142386947","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":"Hollow microporous organic network fiber membrane for efficient extraction of okadaic acid from marine organisms","authors":"","doi":"10.1016/j.chroma.2024.465392","DOIUrl":"10.1016/j.chroma.2024.465392","url":null,"abstract":"<div><div>Membrane-based micro-solid phase extraction (M-μSPE) has garnered great attention in sample pretreatment, suffering an inherent contradiction between permeability and adsorption capacity. In this study, a pure microporous organic network (TEB-DIB-MON) fiber membrane was prepared by combining electrostatic spinning technology, Sonogashira-Hagihara reaction and template sacrifice method. The prepared TEB-DIB-MON membrane exhibited a large specific surface area with a hollow and porous structure, thereby providing excellent solvent permeability and high adsorption capacity for okadaic acid (OA, an algal toxin). Under the optimized conditions, a sensitive analytical method was established by coupling M-μSPE with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The established method has a low detection limit (0.5 pg mL⁻¹), a wide linear range (1.5–1000 pg mL⁻¹, <em>R</em> ≥ 0.9991), and good reproducibility (RSD ≤ 9.4 %, <em>n</em> = 6), which was then successfully applied for OA detection in marine organisms. Trace amounts of OA (59.3–89.0 pg mL⁻¹⁾ was detected in the oyster and prawn samples. This work demonstrated that the excellent application potential of MON membranes in sample pretreatment, while also presents a novel synthesis strategy for MONs membranes.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-10-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142386943","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":"Modification of hollow microporous organic network with polyethyleneimine for efficient enrichment of phenolic acids from fruit juice samples","authors":"","doi":"10.1016/j.chroma.2024.465419","DOIUrl":"10.1016/j.chroma.2024.465419","url":null,"abstract":"<div><div>Owning to the hydrophobic characteristics of microporous organic networks (MONs), their utilizations still largely limited in non- and weak-polar analytes. To expend their applications, here we reported the synthesis of a novel hollowed H-MON-PEI₁₈₀₀–2 composite via sacrifice template method and subsequent modification with polyethyleneimine (PEI) for efficient solid phase extraction of polar and ionic phenolic acid (PAs) from fruit juice samples. H-MON-PEI₁₈₀₀–2 exhibits large surface area, rapid extraction kinetics, remarkable chemical and thermal stabilities, and provides synergistic electrostatic, π-π, hydrogen bonding, and hydrophobic interaction sites for PAs. The developed method owns low limit of detection, wide linear range, large enrichment factors, and good reusability. The recoveries of H-MON-PEI₁₈₀₀–2 for PAs are 1–3 orders of magnitude higher than those of commercial adsorbents like activated carbon, C18 and Oasis HLB. This work highlights the prospects of functional H-MONs for enriching polar and ionic targets from complex sample matrices.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-10-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142386944","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":"Simplified approach to retention times of narrow binary pulses in the case of ideal chromatography model and Langmuir isotherm","authors":"","doi":"10.1016/j.chroma.2024.465405","DOIUrl":"10.1016/j.chroma.2024.465405","url":null,"abstract":"<div><div>Analytical solution to ideal chromatography model has been established for binary Langmuir isotherm and rectangular injections. However, retention time of the less adsorbed species, which is of great theoretical and practical significance, cannot be given in a closed form and is conventionally solved by numerical integration with a floating boundary. A simplified approach is provided in this article. A 4th order algebraic equation was derived and used to solve the maximum concentration that can be further used to explicitly calculate retention time. Under most practical conditions, reliable initial guess can be easily acquired, allowing for the application of Newton-Raphson method for rapid determination of the root of the 4th order equation. In addition, derivatives of retention time with respective to isotherm parameters can be given in analytical forms.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-10-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142386948","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":"Automated kapok fiber-based pipette-tip solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry for rapid and sensitive analysis of tyrosine kinase inhibitors in plasma","authors":"","doi":"10.1016/j.chroma.2024.465420","DOIUrl":"10.1016/j.chroma.2024.465420","url":null,"abstract":"<div><div>This study delineates the development of a novel automated pipette-tip solid-phase extraction (SPE) methodology, employing kapok fiber as a naturally efficient and cost-effective adsorbent for the selective extraction of eleven tyrosine kinase inhibitors (TKIs) from plasma. The uniqueness of this method lies in its assembly, where kapok fibers are ingeniously wrapped around a stainless-steel spring within the pipette tip, ensuring an obstruction-free central space for effortless solution aspiration and dispensation. This design significantly minimizes backpressure, enhancing operational efficiency and ensuring compatibility with pipettors, including the implementation of an electric pipettor to streamline the sample preparation process and facilitate automation. The method's analytical performance, rigorously validated through liquid chromatography-tandem mass spectrometry, exhibits outstanding linearity in ranges of 0.1/0.5–200 ng mL^-1 (R² &gt; 0.993), commendable accuracy (86.3%–114.8%), and consistent precision (3.4–11.3%), alongside remarkably low detection limits that span from 0.024 to 0.130 ng mL^-1. The assembly of kapok fiber within the pipette tip, in this unique configuration, results in a practical, cost-effective, eco-friendly, and automated pipette-tip SPE method. This innovation signifies a significant advancement in bioanalytical methodologies, offering an efficient and sustainable approach for extracting analytes from complex biological samples. This process notably enhances both the sensitivity and selectivity of subsequent instrumental analyses.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8,"publicationDate":"2024-10-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142386940","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}