{"title":"Development and validation of a quantification method for direct oral anticoagulants from capillary blood using volumetric absorptive microsampling and online SPE-LC-MS","authors":"Patrick Opitz, Isabel Waltering, Georg Hempel","doi":"10.1016/j.jchromb.2024.124423","DOIUrl":"10.1016/j.jchromb.2024.124423","url":null,"abstract":"<div><div>The number of prescriptions for new direct oral anticoagulants (DOACs) apixaban, edoxaban, rivaroxaban and dabigatran has increased exponentially in recent years, increasingly replacing the old gold standard, vitamin-K-antagonists. Due to their wide therapeutic range, therapeutic drug monitoring (TDM) is not required, although it has been proven that this could significantly reduce side effects. In order to develop a cost-efficient and simple method for the simultaneous detection of the DOACs and phenprocoumon, a new technology for sample preparation from capillary blood in the ambulant sector named VAMS® was integrated and an LC-MS detector with on-line solid phase extraction (SPE) applying a Turboflow HTLC Cyclone<sup>TM</sup> 1.0x50 mm column was used. The mobile phase consisted of methanol with water (3/97 v/v) and 0.1 % ammonia solution with a flow rate of 2.5 <!--> <!-->mL/min. For the chromatographic separation, a Phenomenex LTD Kinetex 2.6 <!--> <!-->µm C18 100 <!--> <!-->Å, 100x3.0 <!--> <!-->mm column with a flow rate of 0.3 mL/min in gradient mode was utilized. The mobile phase consisted of acetonitrile, water and formic acid (A: 10:90:0.1 v/v and B: 95:05:0.1 v/v). The method was fully validated in the therapeutic range of the substances according to current guidelines. The LLOQ ranged from 3.5 µg/L for rivaroxaban to 88 µg/L for phenprocoumon and the intra-day and inter-day precision was less than 13 % and 12 %, while the accuracy was within a range of 85.7–113 % and 88.7–106 %, respectively. Samples could be stored in the Mitra® devices for at least seven days at room temperature except of dabigatran. Because the Mitras® were used, exactly 10 <!--> <!-->µL of blood could be drawn and no significant haematocrit effect was observed.</div><div>A reliable, simple and cost-effective extraction and analysis LC-MS method could be developed and validated. This method is therefore applicable in ambulatory care.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1251 ","pages":"Article 124423"},"PeriodicalIF":2.8,"publicationDate":"2025-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142833561","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Jialu Zou , Shizhong Zhang , Xiaohong Zhang , Lijuan Xiong , Xuan Chen , Yanmei He , Cancan Duan , Jianyong Zhang
{"title":"Study on the protective mechanism of Xuemaitong Capsule against acute myocardial ischemia rat based on network pharmacology and metabolomics","authors":"Jialu Zou , Shizhong Zhang , Xiaohong Zhang , Lijuan Xiong , Xuan Chen , Yanmei He , Cancan Duan , Jianyong Zhang","doi":"10.1016/j.jchromb.2024.124373","DOIUrl":"10.1016/j.jchromb.2024.124373","url":null,"abstract":"<div><h3>Background</h3><div>Xuemaitong Capsule (XMT) is a widely recognized traditional Miao medicine extensively utilized in Chinese clinical settings. Previous studies have demonstrated XMT protective effects against acute myocardial ischemia (AMI). However, the mechanism by which XMT provides protection to AMI rats is yet to be fully understood.</div></div><div><h3>Aim of the study</h3><div>The purpose of this study was to investigate the protective mechanism of XMT on AMI rats through network pharmacology, traditional pharmacodynamics and metabolomics.</div></div><div><h3>Material and methods</h3><div>The components and potential targets of XMT were identified through the application of traditional Chinese medicine system pharmacology and traditional Chinese medicine molecular mechanism bioinformatics analysis tools. We constructed herb-composition-target networks and analyzed protein–protein interaction (PPI) networks. The potential mechanism was explored by pathway enrichment analysis. Subsequently, the AMI model was constructed by ligation of the anterior descending branch of the left coronary artery, and XMT protective effects on AMI rats were evaluated by analyzing the myocardial enzyme profiles, electrocardiograms<!--> <!-->(ECG), Triphenyltetrazolium chloride<!--> <!-->(TTC) staining, and Hematoxylin-Eosin (HE) staining in AMI rats. Metabolomics based on UHPLC-Q-Exactive Orbitrap MS was used to observe the protective effect of XMT on the serum metabolic profile of AMI, and multivariate statistical analysis further revealed the differential patterns of metabolites after XMT treatment. Finally, integrated pathway analysis was carried out to reveal the biological metabolic mechanism.</div></div><div><h3>Results</h3><div>A total of 392 active components of XMT acted with 624 targets for treating AMI. Pathway enrichment analysis revealed that XMT could treat AMI through TNF, MAPK and PI3K-Akt signaling pathways. Further, XMT could effectively prevent ST-segment elevation in the ECG, reduce the size of myocardial infarction, decrease cardiac weight index and cardiac enzyme levels, and mitigate histological damage in the hearts of AMI rats. In addition, XMT callback 117 metabolites and four metabolic pathways, including taurine and hypotaurine metabolism, phenylalanine metabolism, pyrimidine metabolism and retinol metabolism. Through integrating network pharmacology and metabolomics, we explored the biological mechanism by which XMT treats AMI. It was speculated that the mechanism of XMT is to regulate TNF signaling, PI3K-Akt pathway and MAPK signaling pathway, and participate in cell apoptosis, oxidative stress, immune and inflammatory reaction and other biological processes.</div></div><div><h3>Conclusion</h3><div>XMT plays a protective role in AMI rats by regulating multiple metabolic biomarkers, multiple targets and pathways. Therefore, XMT may provide a potential strategy for the treatment of AMI.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1251 ","pages":"Article 124373"},"PeriodicalIF":2.8,"publicationDate":"2025-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142790813","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yajie Liu , Feng Feng , Xiujuan Wang , Rongzhu Du , Xuesong Feng , Feng Zhang
{"title":"Non-targeted screening of illegal added hypoglycemic drugs and their derivatives in functional foods using characteristic fragment ions scanning based on liquid chromatography-high-resolution mass spectrometry","authors":"Yajie Liu , Feng Feng , Xiujuan Wang , Rongzhu Du , Xuesong Feng , Feng Zhang","doi":"10.1016/j.jchromb.2024.124432","DOIUrl":"10.1016/j.jchromb.2024.124432","url":null,"abstract":"<div><div>Functional foods that are illegally adulterated with chemical hypoglycemic drugs or their derivatives pose serious risks to human health. However, the detection of these compounds is a challenge due to the unknown nature of their structures, particularly as many of these compounds are newly synthesized and lack standardized references. In this study, we developed a non-targeted screening strategy for detecting illegally added hypoglycemic drugs and their derivatives in oral solution and hard capsule functional foods. This strategy utilizes a self-established characteristic fragment ions mass spectrum database based on ultrahigh-performance liquid chromatography–quadrupole/orbitrap high-resolution mass spectrometry. Nine characteristic fragment ions were identified by analyzing the mass spectrometric fragmentation patterns of hypoglycemic drugs. Meanwhile, the precursor and fragment ions of 38 known hypoglycemic drugs were collected and incorporated into the mass database. The detection limits of hypoglycemic drugs in oral solution and hard capsule samples were 0.01–10 μg/L and 0.01–50 μg/kg, respectively. Applying the non-targeted method to 20 batches of suspicious samples, we found that 3 batches of samples contained illegal added drugs. Furthermore, we identified a previously unrecorded hypoglycemic drug not present in the mass database. These results indicate that the developed strategy is a powerful tool for the rapid and highly sensitive identification of both known and unknown hypoglycemic drugs, as well as their derivatives in functional foods.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1251 ","pages":"Article 124432"},"PeriodicalIF":2.8,"publicationDate":"2025-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142870648","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Rafal Typek, Michal P. Dybowski, Michal Rombel, Piotr Holowinski, Andrzej L. Dawidowicz
{"title":"Xenobiotics recovery from plasma using solid phase extraction with C-18 sorbent – The reasons of literature discrepancies","authors":"Rafal Typek, Michal P. Dybowski, Michal Rombel, Piotr Holowinski, Andrzej L. Dawidowicz","doi":"10.1016/j.jchromb.2024.124433","DOIUrl":"10.1016/j.jchromb.2024.124433","url":null,"abstract":"<div><div>Solid phase extraction (SPE) is one of the most popular methods of preparing plasma samples before determining the xenobiotics they contain. The present paper shows that the recovery degree of xenobiotics from plasma samples using SPE with C18 sorbent strongly depends on their storage time and temperature. While xenobiotics can be isolated and recovered in 100 % from fresh plasma samples under optimal conditions of the SPE procedure, their SPE recovery degree from stored plasma is lower. It diminishes with the time increase and temperature reduction of plasma storage. Moreover, a part of xenobiotic in stored plasma samples is not sorbed on SPE-C18 column at all and leaves it together with the waste during loading the column with the examined sample. According to the NMR data, the main reason of the presence of xenobiotics in the waste of the SPE column during its loading are structural-chemical changes occurring in plasma during its storage, leading to the formation of some complex(es) of hydrophilic character with xenobiotic. Another reason for lower SPE recovery degree of xenobiotic from stored plasma is the formation of plasma sediment, which binds/occludes xenobiotic. The presented results expand the current knowledge on why the SPE recovery degree of xenobiotics from plasma reported in the literature may differ. They are important for proper calibration of the chromatographic system in the analysis of xenobiotics in plasma and for achieving high accuracy of the analytical procedure involving SPE in xenobiotic estimation.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1251 ","pages":"Article 124433"},"PeriodicalIF":2.8,"publicationDate":"2025-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142870653","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yuyu Cao , Dayi Xu , Liping Zhang , Kaiyuan Pang , Liyuan Zhang , Xiaobao Wei , Zengxian Sun
{"title":"Determination of four forms of plasma thiol amino acids in individuals with chronic kidney disease by UPLC-MS/MS","authors":"Yuyu Cao , Dayi Xu , Liping Zhang , Kaiyuan Pang , Liyuan Zhang , Xiaobao Wei , Zengxian Sun","doi":"10.1016/j.jchromb.2024.124418","DOIUrl":"10.1016/j.jchromb.2024.124418","url":null,"abstract":"<div><div>The study introduces a robust analytical method based on UPLC-MS/MS for quantifying thiol amino acids, including cysteine (Cys), cysteinylglycine (CG), homocysteine (Hcy), and glutathione (GSH), in their total and total free forms within human plasma. An optimized blank matrix was employed for accurate quantification of endogenous compounds. The method exhibited excellent linearity, precision, accuracy, recovery, and stability, making it highly suitable for plasma analysis. Distinct differences in plasma levels of GSH, Cys, Hcy, and CG across various forms (total, total free, native prototype, and symmetrical oxidation) were observed between healthy individuals and chronic kidney disease (CKD) patients. Comprehensive correlation and receiver operating characteristic (ROC) analyses revealed disrupted thiol amino acid metabolism in CKD, accompanied by heightened oxidative stress. Notably, various forms of Cys and Hcy correlated significantly with renal function markers and demonstrated high diagnostic efficacy in ROC evaluation, with Cys, particularly Cys (F), outperforming others. Hcy further complements Cys in assessing renal function impairment severity.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1251 ","pages":"Article 124418"},"PeriodicalIF":2.8,"publicationDate":"2025-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142890986","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Hongbei Liu , Qiumin Xu , Michael Adu-Frimpong , Yuchu Chen , Ran Li , Fei Xu , Xia Cao , Shanshan Tong
{"title":"In-depth analysis of active compounds targeting tropomyosin-related kinase A via constructed lipid raft @capillary monolith affinity chromatography","authors":"Hongbei Liu , Qiumin Xu , Michael Adu-Frimpong , Yuchu Chen , Ran Li , Fei Xu , Xia Cao , Shanshan Tong","doi":"10.1016/j.jchromb.2024.124429","DOIUrl":"10.1016/j.jchromb.2024.124429","url":null,"abstract":"<div><div>In order to enrich the selection of biological ligands, realize the miniaturization analysis, and broaden the application of monolith materials for active ingredients screening and separating, we sough to construct a lipid raft @capillary monolith microcolumn affinity chromatography model. Single factor experiments and various characterization methods, including scanning electron microscopy (SEM) and thermogravimetric analysis, were employed to investigate the polymerization of the monolith column under different material ratios to determine optimal preparation conditions. Subsequently, the lipid raft from U251 cells was integrated with the monolith materials based on epoxy-based covalent crosslinking principle and characterized through SEM and immunofluorescence methods. Afterwards, the retention of positive drug gefitinib, negative drug gemcitabine and four licorice standards solution on the prepared lipid raft monolith microcolumn was then detected via electrochemical detection. The results exhibited that there was no specific adsorption for any active compounds on the blank monolith materials. Significantly, the lipid raft monolith microcolumn packed with TrkA-target proteins could be successfully validated for positive drug gefitinib with a high affinity sorption efficiency of 51.2%. This work expands the range of the utilization of affinity chromatography carriers and the selection of biological ligands, providing a new idea for the screening of active ingredients.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1251 ","pages":"Article 124429"},"PeriodicalIF":2.8,"publicationDate":"2025-01-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142890991","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Faten Farouk , Marwa Sharaky , Ehab F. Elkady , Rawda M. Sayed
{"title":"Chromatographic retention assisted in-silico prediction of anticancer potential of glucocorticoids on cancer cell lines","authors":"Faten Farouk , Marwa Sharaky , Ehab F. Elkady , Rawda M. Sayed","doi":"10.1016/j.jchromb.2025.124466","DOIUrl":"10.1016/j.jchromb.2025.124466","url":null,"abstract":"<div><div>Glucocorticoids (GCs) are hallmarks of anti-inflammatory activity. They are used as adjuvant therapy in oncology medications to alleviate some of the associated side effects. Although recent research has indicated that GCs have favorable anticancer potential, some scientific evidence suggests a pro-proliferation impact of GCs on cancer cells. This may create a scientific confusion on the utility of GCs and the choice of which GC enhances the anticancer potential and mitigates the negative effect. Accurate <em>in-silico</em> prediction and correct ranking of biological activity may be limited by the impact of the physicochemical interaction between small molecules and biological membranes. Chromatographic retention is inherently dependent on the physicochemical properties of the test molecule. It can scale the relative hydrophobicity and tentatively indicate the membrane permeability. In this study, the relationship between the <em>in-silico</em> binding affinity, the chromatographic retention and the <em>in-vitro</em> anticancer activity was investigated. Fifteen GCs were chromatographically separated on an Inertsil® C18 (4.6 * 250 mm; 5 μm) HPLC column. The binding affinity of the test GCs was determined on three receptors involved in cancer cell proliferation (topoisomerase II (TOPII), glucocorticoid receptor (GR) and ATP-binding cassette (ABCG2)). The antiproliferative potential of the test steroids was determined as per their IC<sub>50</sub>. The correlation between chromatographic retention and the binding affinity to the observed IC<sub>50</sub> was investigated by multiple linear regression (MLR). Results revealed that some GCs exhibited a remarkably favorable inhibitory potential against cancer cell lines over normal cell lines. Our data indicated a significant correlation between the retention times of different GCs and the determined binding affinity, especially to the GR (r<sup>2</sup> = 0.677; <em>p</em> = 0.011) and the estrone sulphate (ESS) binding site of the ABCG2 (r<sup>2</sup> = 0.643; <em>p</em> = 0.018). Concurrently, the retention times were well correlated to the observed IC<sub>50</sub> on the colorectal cancer cell lines (r<sup>2</sup> = 0.580; <em>p</em> = 0.038) and the hypopharyngeal cell lines (r<sup>2</sup> = 0.638; <em>p</em> = 0.019). Significant MLR models (n = 4) correlating the retention times of the tested steroids and the binding affinity to the observed IC<u><sub>50</sub></u> were created. The MLR model correlating the retention times and the ABCG2_ESS binding affinity to the IC<sub>50</sub> on lung cancer was the most significant (<em>p</em> = 0.004). The accuracy of the model was 107.12 ± 29.18 % indicating good IC<sub>50</sub> prediction abilities.</div><div>In conclusion, chromatographic retention can be employed as a low-cost and simple auxiliary tool for improving the <em>in-silico</em> prediction of the <em>in-vitro</em> activities of small molecules.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1253 ","pages":"Article 124466"},"PeriodicalIF":2.8,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143035706","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yuanxiao Wang , Xueying Chen , Feifan Zhou , Mingyu Pan , Yanjiao Huang , Makoto Tsunoda , Yingxia Zhang , Haimei Yang , Lu-shuang Li , Yanting Song
{"title":"Bidirectional transport studies of flavonoids from Alpiniae oxyphyllae fructus by in vitro inflammatory blood–brain barrier model combined with UHPLC-MS/MS analysis","authors":"Yuanxiao Wang , Xueying Chen , Feifan Zhou , Mingyu Pan , Yanjiao Huang , Makoto Tsunoda , Yingxia Zhang , Haimei Yang , Lu-shuang Li , Yanting Song","doi":"10.1016/j.jchromb.2025.124471","DOIUrl":"10.1016/j.jchromb.2025.124471","url":null,"abstract":"<div><div><em>Alpiniae oxyphyllae</em> fructus (AOF) has been widely used for the treatment of central nervous system (CNS) diseases. Flavonoids, namely, baicalein, wogonin, and pinocembrin, are bioactive components with neuroprotective effects against AOF. Herein, a lipopolysaccharide (LPS)-induced in vitro inflammatory blood–brain barrier (BBB) model of a co-culture of hCMEC/D3 and HA1800 cells was constructed to investigate the permeability of flavonoids. The values of transmembrane resistance (TEER), apparent permeability (<em>P</em><sub>app</sub>) of sodium fluorescein (Na-F), and levels of TNF-α and IL-1β confirmed the construction of the in vitro inflammatory BBB model. An ultra-high-performance liquid chromatography–mass spectrometry (UHPLC-MS/MS) was established to quantify the permeability of the three flavonoids. The average coefficients (R<sup>2</sup>) of the calibration curves were better than 0.99. The intraday and interday accuracies ranged from −13.75 % to 6.37 % and −14.28 % to 11.80 %, respectively. The recoveries and matrix effects were higher than 88.00 % and 92.42 %, respectively. These results indicated that the methodology was reliable. Compared with the normal BBB model, the permeability and efflux ratios of the three flavonoids significantly increased using the inflammatory BBB model. <em>P</em><sub>app BL→AP</sub> of wogonin and pinocembrin increased by approximately 1.3 and 5.5 times, respectively, thereby increasing the efflux ratios by 48 % and 76 %, respectively. The efflux ratios of the three flavonoids in the AOF were all < 2, demonstrating that they passed through the BBB in a passive diffusion way. This study investigated flavonoid transport from the AOF using the in vitro inflammatory BBB model, providing a material basis for neuroprotection as a potential drug for treating CNS diseases.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1253 ","pages":"Article 124471"},"PeriodicalIF":2.8,"publicationDate":"2025-01-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143073091","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Laura Reyes , Caroline Bourgeois , Guillaume Gautier Renard , Patrick Jame , Xavier Saupin , Clémence Nikitine , Léa Vilcocq
{"title":"Analysis of aliphatic and phenolic compounds present in industrial black liquors using HPLC-DAD and IC-MS/MS methods","authors":"Laura Reyes , Caroline Bourgeois , Guillaume Gautier Renard , Patrick Jame , Xavier Saupin , Clémence Nikitine , Léa Vilcocq","doi":"10.1016/j.jchromb.2024.124442","DOIUrl":"10.1016/j.jchromb.2024.124442","url":null,"abstract":"<div><div>Carboxylic acids and aromatic compounds are essential building blocks and starting materials for the production of a wide range of fine chemicals and materials. Their recovery from kraft black liquor, an industrial effluent from pulp and paper mills, is a promising way to produce alternative bio-based chemicals. Reliable methods are needed to identify and quantify the molecules of interest in complex mixtures such as black liquors. First, an HPLC-DAD-based method was developed for the determination of aliphatic acids and phenolic compounds. It allowed the separation of 31 aliphatic and phenolic compounds. The method was applied to the identification of aliphatic and phenolic compounds in industrial black liquors. Then, an IC-MS/MS method was developed to confirm the identification and quantification of organic compounds in black liquor samples. 22 compounds were detected and identified by MS/MS detection.</div><div>According to both methods, the major aliphatic acids in softwood kraft black liquor are formic acid (9.8 g/L), acetic acid (7.1 g/L), lactic acid (5.2 g/L), glycolic acid (4.7 g/L), 2-hydroxybutyric acid (2.3 g/L), and oxalic acid (1.3 g/L). Phenolic compounds were detected at very low levels (total concentration 1.4 g/L). This study demonstrates the value of a multi-technique strategy for the identification and quantification of organic compounds in complex matrices such as black liquor.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1253 ","pages":"Article 124442"},"PeriodicalIF":2.8,"publicationDate":"2025-01-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143027485","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yingying Pan , Zihan Tan , Ping Liu , Aixia Yang , Lin-Lin Chen
{"title":"Corrigendum to “Pharmacokinetic and tissue distribution study of pectolinarigenin in rats using UPLC-MS/MS” [J. Chromatogr. B 1247 (2024) 124344]","authors":"Yingying Pan , Zihan Tan , Ping Liu , Aixia Yang , Lin-Lin Chen","doi":"10.1016/j.jchromb.2024.124366","DOIUrl":"10.1016/j.jchromb.2024.124366","url":null,"abstract":"","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1250 ","pages":"Article 124366"},"PeriodicalIF":2.8,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142581352","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}