Journal of separation science最新文献

{"title":"Quantification of Epigenetic DNA and RNA Modifications by UHPLC–MS/MS Technologies: New Concepts and New Improvements for the Special Collections","authors":"Rui Zhang,&nbsp;Hailong Liu,&nbsp;Biao Bai,&nbsp;Hailin Wang","doi":"10.1002/jssc.70159","DOIUrl":"https://doi.org/10.1002/jssc.70159","url":null,"abstract":"<div>\u0000 \u0000 <p>Dynamic and reversible DNA and RNA modifications are essential for cell differentiation and development. Aberrant epigenetic modifications are closely associated with the occurrence and progression of diseases, serving as potential markers for cancer diagnosis and prognosis. Ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UHPLC–MS/MS) offers distinct advantages in the qualitative and quantitative analysis of various modifications due to its sensitivity, specificity, and accuracy. This review provides a comprehensive overview of the current knowledge regarding the liquid chromatography–mass spectrometry (LC–MS) analysis of DNA and RNA modifications, including analytical procedures, advancements, and biological applications, with a focus on tracing the source of (N6-2′-deoxy-adenosine) 6mdA in eukaryotes. Additionally, we examine the integration of UHPLC–MS/MS with other separation techniques to achieve accurate quantification of modifications in specific regions, certain fragments, and free nucleosides.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143925973","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Qualitative Analysis of Chemical Components in Shiqi Waigan Granules Using UHPLC-QTOF/MS and GC-MS Technologies","authors":"Lin Feng,&nbsp;Xiaokang Liu,&nbsp;Ling Li,&nbsp;Ling Fang,&nbsp;Yaling An,&nbsp;Zijun Tang,&nbsp;Yushi Huang,&nbsp;Zhenwei Li,&nbsp;Lihua Peng,&nbsp;Weilin Qiao,&nbsp;De-An Guo","doi":"10.1002/jssc.70144","DOIUrl":"https://doi.org/10.1002/jssc.70144","url":null,"abstract":"<div>\u0000 \u0000 <p>Shiqi Waigan granules (SWG) are indicated for the treatment of fever and headache associated with external pathogenic cold, as well as for the prevention of influenza. However, due to its complex composition, little attention has been given to the analysis of chemical components present in SWG. This study employs ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-QTOF/MS) combined with gas chromatography-mass spectrometry (GC-MS) to provide a reliable and comprehensive method for characterizing the chemical components in SWG. By screening with high mass accuracy (&lt; 10 ppm) and comparing with literature and UHPLC-MS/MS online databases, the fragmentation pathways and characteristic fragments of some representative compounds were elucidated. A total of 138 compounds were successfully identified, including flavonoids, phenylpropanoids, organic acids, phenols, lignans, nucleosides, terpenoids, glycosides, and other plant chemicals. Then, the volatile compounds in SWG were characterized using GC-MS combined with the NIST library, and a total of 14 compounds were putatively characterized. These findings not only help elucidate the material basis of the pharmacological actions of SWG, providing the necessary basis for the quality control and standardization of SWG, but also offer references for the separation of small-molecule compounds. The science of traditional Chinese medicine separation is shifting from a “single-component orientation” to a focus that balances “holism and precision.” Modern technologies have significantly enhanced the efficiency and quality control of component separation.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143919860","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Isolating and Purification Technologies for Glycyrrhizic Acid","authors":"Meng Zhao,&nbsp;Qing Wang,&nbsp;Yun Yang,&nbsp;Lanlan Sun,&nbsp;Xue-Song Gu,&nbsp;Chang-Jiang-Sheng Lai","doi":"10.1002/jssc.70165","DOIUrl":"https://doi.org/10.1002/jssc.70165","url":null,"abstract":"<div>\u0000 \u0000 <p>Glycyrrhizic acid (GA) is the primary active component of the traditional Chinese medicinal herb licorice. It possesses antimicrobial, anti-inflammatory, and antitumor activities. In addition, due to its unique sweetness, it can also be used as a food additive. Traditional Chinese medicines are typically used directly as drugs. However, the chemical composition of Chinese medicinal materials such as licorice is complex, containing not only effective components but also ineffective and even toxic substances. To efficiently exert their medicinal value and minimize the side effects of harmful substances, the extraction and separation of the active components is an important means to achieve the modernization of traditional Chinese medicine utilization. This article focuses on the extraction of GA, summarizes the current technologies related to the extraction and separation of GA, reveals the underlying chemical principles, and evaluates the advantages and disadvantages of the corresponding technologies. On this basis, it proposes challenges faced in the separation of GA and provides corresponding solutions. The author believes that with the continuous introduction of precise chemical synthesis and other methods in separation, the extraction and separation of the active substance will become greener and more efficient. It will also provide a reference for the extraction of other effective components of traditional Chinese medicine.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143925974","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Recent Developments in Deep Eutectic Solvents Applications in Liquid Chromatography: 2019–2025","authors":"Derya Demir,&nbsp;Joanna Antos,&nbsp;František Švec,&nbsp;Hana Sklenářová","doi":"10.1002/jssc.70160","DOIUrl":"https://doi.org/10.1002/jssc.70160","url":null,"abstract":"<p>Deep eutectic solvents (DES) are used as mobile phase and stationary phase modifiers, or as for the stationary phase itself for thin layer/liquid/supercritical chromatography. Their specific properties can improve the separation selectivity, reduce peak tailing, and shorten the separation time. In terms of environmental impact, the advantages of DES are based on their biodegradability, recyclability, and stability in terms of mechanical/chemical/thermal properties. The disadvantages are related to higher viscosity and degradation in aqueous solutions. This review focuses on works that have been published since 2019, the year the excellent comprehensive review by Cai and Qiu was printed. Selected parameters are discussed that should be considered when DES are preferred over commonly used mobile and stationary phases due to green chemistry trends, while taking into account their limitations in modern LC separations. This review also centres on critical aspects of DES applications in the field of liquid and supercritical fluid chromatographic separations.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70160","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143914575","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A Protocol for Conformity and Risk Assessment of Pharmaceutical Product by High Performance Liquid Chromatography Based on Measurement Uncertainty","authors":"Zhong Xue,&nbsp;Xuening Mou,&nbsp;Hao Sun,&nbsp;Chunqi Cao,&nbsp;Bing Xu","doi":"10.1002/jssc.70158","DOIUrl":"https://doi.org/10.1002/jssc.70158","url":null,"abstract":"<div>\u0000 \u0000 <p>Conformity assessment plays a critical role in the process of drug manufacturing, significantly influencing product outcomes of acceptance or rejection. Measurement uncertainty is an important parameter inherent to the analysis method itself. The introduction of uncertainty can effectively control and assess the risk of making wrong decisions in the conformity assessment process. This protocol provides guidelines for conformity and risk assessment of pharmaceutical products based on measurement uncertainty. The procedure is successfully applied to the HPLC analytical method of determination of berberine hydrochloride in Daochi pills. The correlation coefficient (<i>r</i>) of berberine hydrochloride was 0.9999, which indicated a good linear relationship within the range of 0.02317∼2.317 ug·mL⁻¹. The validation experiment adopted an experimental design of 3 replicates × 3 days × 3 concentrations. The results showed the accuracy as mean recovery was 100.29% with repeatability of 1.72% and intermediate precision of 1.76% (<i>n</i> = 27). And the relative expanded uncertainty of the HPLC method was 4.04%. Furthermore, the acceptable limit of the content of berberine hydrochloride in Daochi pills was calculated for the conformity assessment. The risk assessment was accomplished by the Monte Carlo simulation, with the customer risk and producer risk as 3.64% and 5.89%, respectively.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143914456","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Chemical Characterization of the Traditional Chinese Medicine Zishui Qingxin Yin by Ultra-High Performance Liquid Chromatography and Q Exactive Orbitrap Mass Spectrometers Combined With Molecular Networking and Quantitative Analysis of the Main Components by High-Performance Liquid Chromatography With Diode Array Detection","authors":"Fei Pang,&nbsp;Yi-Wei Zhou,&nbsp;Ying-Chu Shi,&nbsp;Yu-Xin Yu,&nbsp;Jiu-Xia Gao,&nbsp;Ling Zhang,&nbsp;Jia Xu","doi":"10.1002/jssc.70166","DOIUrl":"https://doi.org/10.1002/jssc.70166","url":null,"abstract":"<div>\u0000 \u0000 <p>Atopic dermatitis is a recurrent, pruritic, localized eczema. <i>Zishui Qingxin Yin</i> (ZSQXY) is derived from two classic prescriptions, Daochi San and Bao He Wan, and has a significant antipruritic effect in clinical practice, but the pharmacodynamic material basis of its action is still unclear. In this study, ultra-high performance liquid chromatography and Q Exactive Orbitrap mass spectrometers combined with Molecular Networking method was established to comprehensively analyze its chemical components. A total of 247 chemical compounds were identified, of which 12 were new compounds; the structural types included 89 flavonoids, 54 terpenoids, 56 alkaloids, 39 phenylpropanoids, and 18 other compounds, and the identified compounds were classified into different traditional Chinese medicines. At the same time, high-performance liquid chromatography with diode array detection was used to determine the content of 14 compounds with higher contents in ZSQXY. This study provides a scientific basis for further studying the mechanism of action, metabolic characteristics, and subsequent development of ZSQXY.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143909049","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Digital Restoration of Separations Data","authors":"M. Farooq Wahab,&nbsp;Troy T. Handlovic","doi":"10.1002/jssc.70139","DOIUrl":"https://doi.org/10.1002/jssc.70139","url":null,"abstract":"<div>\u0000 \u0000 <p>In experimental separations, the acquired signal can have four common but unwanted elements: (i) high-frequency noise, (ii) drift, (iii) occasional periodic and pink noise, and (iv) a mixture of components traveling with close velocities. Additionally, separation scientists observe partially resolved peaks in chromatographic or capillary electrophoresis detector output. A protocol for digitally recovering the “true data” is provided with clear-cut details and open-access codes for formulating denoising, baseline correction, and peak resolution problems as linear or nonlinear optimizations. The smoother of Bohlmann–Whittaker denoises and preserves the total area of the signal. Fourier transform methods to detect and remove periodic noise are also proposed for erratic periodic noise problems. A peak width preserving filter, called the bilateral filter, is also given. This procedure is followed by two reliable baseline correction algorithms based on asymmetric reweighted least squares or curvature-based weights to deal with low-frequency signal variations. Once low- and high-frequency noise components are removed, a convenient peak mode location method is introduced, relying upon numerically stable second derivative calculation from Savitzky–Golay (SG) filter. Peak locations, area, height, and higher statistical moments can be derived from iterative curve fitting. The protocol shows two peak models that can model left or right skewed peaks. The new peak models are (i) a numerically stable version of the bi-directional exponentially modified Gaussian (EMG), suitable for a wide variety of real chromatograms, and (ii) the twice generalized normal model with third- and fourth-moment parameters built into it. The nonlinear least squares regression approach uses the trust-region reflective optimization method. The algorithm converges to a solution even with multiple peaks and approximate guesses of peak parameters. The protocol can be generalized to fit more than 200 peak functions in separation sciences available in literature by minor adaptations of the provided codes in the MATLAB environment.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143909051","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Biomonitoring Livestock Antiparasitic Residues: Development of Fast Mass Spectrometric Methods for the Quantification of Ivermectin, Albendazole, and their Metabolites in Sheep Plasma and Feces","authors":"Theodora E. Barmpouni,&nbsp;Athanasios I. Gelasakis,&nbsp;Eirini Tsimpouri,&nbsp;Serkos A. Haroutounian,&nbsp;Kyriaki Machera,&nbsp;Konstantinos M. Kasiotis","doi":"10.1002/jssc.70156","DOIUrl":"https://doi.org/10.1002/jssc.70156","url":null,"abstract":"<div>\u0000 \u0000 <p>Antiparasitic substances are extensively used in livestock farming against common parasitic infections. Improper utilization of these medicines often leads to the development of antiparasitic resistance and the detection of residues across the food chain, posing significant challenges to animal health, food safety, and public health. The objective of this study was to monitor antiparasitics’ pharmacokinetics after the administration of ivermectin and albendazole in farm sheep. To achieve this goal, a fast LC-ESI-MS/MS method was developed and validated for the simultaneous quantification of ivermectin, albendazole, and their metabolites in sheep plasma. Concurrently, a probe electrospray tandem mass spectrometry ultrafast method was also developed for the real-time monitoring of albendazole and its metabolites in plasma. In addition, the liquid chromatography methodology was extended and validated for the detection of ivermectin in sheep feces, offering a non-invasive alternative to tissue and biofluids analysis. The detection capability values estimated for the techniques developed herein for the studied compounds and their metabolites in plasma ranged from 0.1 to 50.2 ng/mL, while the respective values for ivermectin in feces ranged between 5.0 and 26.9 ng/g. Recoveries fluctuated from 64% to 119%, proving the competence of the methods. The application of these methods in sheep samples, after the administration of the antiparasitic substances, effectively indicated the distribution of their concentrations, although in some cases, the individual animal effect seemed to interplay with the expected results. Also, these methods can contribute to the adjustment of the farm animal antiparasitic protocols, promoting the most effective utilization of the respective drugs while minimizing the risk of developing antiparasitic resistance. In a broader context, they may aid the advancement of veterinary medicine, offering practical solutions for monitoring the drug residues in farm animals and the derived products, and mitigating the risks associated with the extensive and uncontrolled utilization of antiparasitic drugs.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143908909","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A HILIC-IM-MS-Based Pharmacometabodynamic Study of the Effects of Orally Administered Gefitinib on the Polar Urinary Metabolic Phenotypes of C57Bl6 Mice","authors":"Adam King,&nbsp;Lee A. Gethings,&nbsp;Robert S. Plumb,&nbsp;Ian D. Wilson","doi":"10.1002/jssc.70163","DOIUrl":"https://doi.org/10.1002/jssc.70163","url":null,"abstract":"<p>The effects of the anilinoquinazoline tyrosine kinase inhibitor (TKI) gefitinib on the polar urinary metabolome of mice following oral administration (50 mg/kg) were studied over the 24 h period post dose. Analysis was performed using a hydrophilic interaction liquid chromatographic separation (HILIC) hyphenated to cyclic ion mobility (cIM) and mass spectrometry (MS). This investigation revealed numerous time-dependent changes in the polar urinary metabolic phenotype of gefitinib-dosed mice that mirrored the plasma concentrations and urinary excretion of the drug and its metabolites. These changes showed both relative increases and decreases in the amounts of various endogenous metabolites, including 8-hydroxydeoxyguanosine, thymidine, acetylcarnitine, isobutyrylcarnitine, myristoylglycine, 3-phenylpropionylglycine, cyclic AMP, 19-oxotestosterone, and 3′-asparagine-AMP. These changes were generally seen to be greatest at the time of the highest plasma and urinary concentrations of gefitinib. The concordance of these effects on the urinary metabolome with plasma/urine drug concentrations strongly implies a range of pharmacometabodynamic effects pointing to mechanism-based regulation of a number of endogenous metabolic pathways by gefitinib.</p>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/jssc.70163","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143909050","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Separation and Quantification of Cyclic di-AMP, -GMP, and Cyclic GAMP in Bacteria Using LC–MS/MS","authors":"Silvio Uhlig,&nbsp;Kristina Vevik,&nbsp;Joke Van De Vyver,&nbsp;Inger Sofie Dragland,&nbsp;Lene A. Grutle,&nbsp;Maria Pain,&nbsp;Roger Simm","doi":"10.1002/jssc.70157","DOIUrl":"https://doi.org/10.1002/jssc.70157","url":null,"abstract":"<div>\u0000 \u0000 <p>This study summarizes the optimization of a selective method for UHPLC-separation and subsequent tandem mass spectrometric detection of adenosyl- and guanosyl-containing cyclic dinucleotides in bacteria. Cyclic dinucleotides are a class of bacterial second messenger molecules, and their cellular concentrations are tightly regulated by biosynthesis and enzymatic breakdown. Although bacteria, according to present knowledge, only produce 3′,3′-linked cyclic dinucleotides, other nucleotide variants also exist, including structural isomers, which may lead to misidentifications. Mixtures of the 2′,2′-, 2′,3′-, and 3′,3′-linked isomers of cyclic di-AMP, cyclic di-GMP, and cyclic GAMP were separated using an octadecylsilane-amide column. Subsequent tandem mass spectrometric detection was based on monitoring the adenosyl- or guanosyl-product ions for quantification, and additional monitoring of up to three product ions for verification. We show the presence of an unidentified putative structural isomer of cyclic di-AMP in several bacterial species. Cyclic di-AMP was quantified using an isotope dilution approach and ¹⁵N₁₀-cyclic di-AMP as an internal standard, whereas instrument calibration for other variants was performed using matrix-matched calibration. The combined measurement uncertainty u′ for the quantification of the nine cyclic dinucleotide variants in anion-exchanged bacterial extracts was 10%–41%, determined at an extract concentration of 12 nM. Our study also demonstrated the application of total protein measurements in resuspended, nucleotide-extracted, bacterial pellets to normalize nucleotide concentrations.</p>\u0000 </div>","PeriodicalId":17098,"journal":{"name":"Journal of separation science","volume":"48 5","pages":""},"PeriodicalIF":2.8,"publicationDate":"2025-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143901081","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}