Se pu = Chinese journal of chromatography最新文献

{"title":"[Determination of atmospheric intermediate volatility organic compounds with thermal desorption-flow modulator comprehensive two-dimensional gas chromatography- time-of-flight mass spectrometry].","authors":"Rui Wang, Ying-Jie Li, Jia-Hua Wang, Chang-Wen Ma, Jia-Kui Jiang","doi":"10.3724/SP.J.1123.2025.07009","DOIUrl":"10.3724/SP.J.1123.2025.07009","url":null,"abstract":"<p><p>Atmospheric intermediate volatile organic compounds （IVOCs） are complex mixtures. Due to the limited separation and identification capabilities of one-dimensional gas chromatography （<sup>1</sup>D-GC）， a large portion of atmospheric IVOCs-which often elute as unresolved or complex peaks-are categorized as an unspeciated complex mixture （UCM）. This constrains the accurate apportionment of atmospheric IVOCs. To address this problem， an alternative analytical method has been developed utilizing thermal desorption-flow modulation comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry （TD-FM GC×GC-TOF MS） to measure atmospheric IVOCs. Analytical optimization focused on fill and flush time within a 3-second modulation period， with optimal values determined as 2 870 ms and 130 ms， respectively， to maximize separation efficiency and signal response. Compounds were separated on a ZB-5HT column （20 m×0.18 mm×0.18 μm） as the first dimension， with a BP-50 column （5 m×0.25 mm×0.20 μm） serving as the second dimension. Helium was employed as the carrier gas with column pressures maintained at 254.4 kPa （first dimension） and 202.1 kPa （second dimension）. The following temperature program was used： 50 ℃ for 10 min， then increased to 300 ℃ at 10 ℃/min， with the final temperature held for 20 min. The MS was operated in electron impact （EI， 70 eV） ionization mode. Both the ion source and transfer line temperatures were set at 300 ℃. MS signals were recorded in full scan mode with a scan range of <i>m/z</i> 40 to <i>m/z</i> 800. During thermal desorption， the desorption temperature was set at 320 ℃， and the cold trap temperature was maintained at -10 ℃ to capture desorbed targets. The secondary desorption flow rate was set at 16 mL/min. Under these optimized conditions， the method demonstrated acceptable linearity， with correlation coefficients ranging from 0.922 3 to 0.998 4， for 69 selected targets spanning 1 to 20 ng/tube， with method detection limits （spiked at 1 ng/tube） between 0.010 7 and 0.410 1 ng/m<sup>3</sup>， with recoveries ranging from 80.4% to 136.0%. Relative standard deviation values among replicate samples （<i>n</i>=7） spiked at 1 ng/tube， 3 ng/tube， and 10 ng/tube levels were around 4.5%-33.9%， 3.2%-19.9% and 3.5%-18.6%， respectively. Application of the method to atmospheric IVOC samples collected from an urban site of Shanghai， revealed total IVOCs mass concentrations of 8.6-61.1 μg/m<sup>3</sup>. Of these， mass concentrations of 853 individual species identified by the present method comprised 96.2% of total IVOCs. Consequently，the newly developed method improved the identification rate for UCM. Importantly， the newly speciated aromatics， chlorinated IVOCs， and oxygenated IVOCs exhibited different emission sources distinct from those routinely monitored compounds. Therefore， this study established a reliable method for determining atmospheric IVOCs， offering strong data support for precise source appo","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 4","pages":"453-466"},"PeriodicalIF":0.0,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13077543/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147680127","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Magnetic fluorinated covalent triazine frameworks for efficient extraction of perfluorinated compounds].","authors":"Wen-Min Zhang, Guan-Cheng Liu, Min Fang, Jun-Ling Guo, Lan Zhang","doi":"10.3724/SP.J.1123.2025.07004","DOIUrl":"10.3724/SP.J.1123.2025.07004","url":null,"abstract":"<p><p>Perfluorinated compounds （PFCs） are a new type of persistent organic pollutants. When consumers consume soft drinks contaminated with PFCs， it can cause severe systemic diseases. Increasing concern regarding the presence of PFCs in soft drinks has resulted in the need for reliable analytical methods for the monitoring of PFCs. However， the content of PFCs in soft drinks is extremely low and the matrix is complex， making it difficult to directly determine their content using high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）. Therefore， the necessary sample pretreatment is required before instrumental analysis. Magnetic solid-phase extraction （MSPE） is a simple， rapid， and efficient solid-liquid separation technique， and its extraction efficiency depends on the characteristics of the magnetic adsorbent. Covalent triazine frameworks （CTFs） are porous organic polymers connected by triazine bonds. They have the characteristics of large specific surface area， rich pore structure， adjustable functionality， good chemical stability and thermal stability， making them widely used in sample pretreatment. In this study， a magnetic fluorinated covalent triazine framework material （Fe<sub>2</sub>O<sub>3</sub>/CTF-F） was prepared by a one-pot method and characterized in detail. The X-ray photoelectron spectra （XPS）， Fourier-transform infrared （FT-IR） spectrum， and X-ray diffraction （XRD） pattern demonstrated the successful synthesis of Fe<sub>2</sub>O<sub>3</sub>/CTF-F with a high fluorine content （17.50%）， which was formed through tetrafluoroterephthalonitrile polymerization and hydrated ferric chloride decomposition. The highly fluorinated material can provide a specific and strong affinity for PFCs through fluorous-fluorous （F-F） interactions. The experimental results of nitrogen adsorption-desorption and magnetic properties showed that the Fe<sub>2</sub>O<sub>3</sub>/CTF-F has a high specific surface area （1 452.3 m<sup>2</sup>/g） and porosity （0.82 cm<sup>3</sup>/g）， as well as a strong magnetic responsivity （7.1 emu/g）. It indicates that the Fe<sub>2</sub>O<sub>3</sub>/CTF-F possesses a large number of accessible adsorption sites and a rapid magnetic separation capability， providing a guarantee for efficient extraction of PFCs. Subsequently， the Fe<sub>2</sub>O<sub>3</sub>/CTF-F was used as an adsorbent for MSPE technology for the efficient extraction of seven PFCs. Because of its many accessible adsorption sites and strong fluorine-fluorine interactions， the Fe<sub>2</sub>O<sub>3</sub>/CTF-F showed excellent extraction ability for PFCs. Finally， by combining the MSPE method with HPLC-MS/MS technology， a new analytical method was established for the analysis of PFCs in soft drinks. To achieve the best performance， single-factor experiments were conducted to optimize the dosage of the adsorbent， the extraction time， the elution solvent and elution time in the MSPE process. Under the optimal conditions， the established analyt","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 4","pages":"383-392"},"PeriodicalIF":0.0,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13077536/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147680119","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Determination of ergot alkaloids toxins in forage grass by ultra performance liquid chromatography-tandem mass spectrometry coupled with solid-phase supported liquid-liquid extraction].","authors":"Cai-Xia Ren, Xiao-Min Wang, Wan-Li Sheng, Yi-Zhi Han, Chun-Yan Zhang, Shu-Zhan Zheng","doi":"10.3724/SP.J.1123.2025.02014","DOIUrl":"10.3724/SP.J.1123.2025.02014","url":null,"abstract":"<p><p>Toxic alkaloids， especially ergot alkaloid toxins， present in forage grass and pose serious health hazards to humans and livestock. Hence， a method for simultaneously detecting these dangerous plant toxins is needed. This study established a rapid method for detecting ten ergot alkaloid toxins using solid-phase supported liquid-liquid extraction technology combined with ultra performance liquid chromatography-tandem mass spectrometry. Forage samples were extracted with 8.0 mL of acetonitrile containing 1% formic acid. The extraction mixture was vortexed and then centrifuged at 8 000 r/min for 5 min， after which 1.0 mL of the supernatant was mixed with 3.0 mL of water and vortexed for 0.5 min. The entire mixture was transferred to a solid-phase supported liquid-liquid extraction column and allowed to stand for 10 min. The column was eluted with 6.0 mL of ethyl acetate and the collected eluate was evaporated under nitrogen at temperatures below 40 ℃. The residue was dissolved in 1 mL of acetonitrile-water （1∶3， volume ratio， containing 0.5% formic acid）， and separated using an Acquity UPLC BEH C<sub>18</sub> column （100 mm×2.1 mm， 1.7 μm）. A solution of 0.5% formic acid in water containing 0.25 mmol/L ammonium acetate was used as mobile phase A， while 0.5% formic acid in acetonitrile was used as mobile phase B. The following gradient elution program was used： 0-1.0 min， 90%B； 1.0-5.0 min， 90%B-75%B； 5.0-10 min， 75%B-50%B； 10-12 min， 50%B-10%B； 12-14 min， 10%B； 14-16 min， 10%B-90%B. Ten ergot alkaloid toxins （including three pairs of isomers： ergocornine， ergocristine， ergocristinine， ergocryptine， and ergocryptinine） were effectively separated following gradient elution. Positive electrospray-ionization mode and multiple reaction monitoring （MRM） scanning was used for detection， with an external standard curve used for quantification purposes. The ten ergot alkaloid toxins exhibited good linear relationships within their respective linear ranges （<i>r</i><sup>2</sup>>0.995）. Alfalfa， <i>Leymus chinensis</i>， oats， and silage corn exhibited LODs of 0.1-2.3 μg/kg for the ten ergot alkaloid toxins， with LOQs of 0.4-7.3 μg/kg. The developed method exhibited overall recovery rates of between 66.3% and 116.7%， with relative standard deviations of less than 9.9%. The matrix effect mainly manifested itself in the form of matrix suppression， with silage corn exhibiting a significantly stronger matrix effect than the other three types of forage. Silage corn exhibited a strong matrix effect in more than 50% of samples， while alfalfa， oats， and <i>Leymus chinensis</i> showed relatively low matrix effects， with more than 63% being weak. The developed method is simple to operate， provides accurate results， and exhibits minimal interference； hence， it is suitable for simultaneously screening and confirming ergot alkaloid toxins in forage， thereby providing technical support for monitoring forage quality， while also expanding the applicability of solid-phase","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 4","pages":"403-412"},"PeriodicalIF":0.0,"publicationDate":"2026-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13077538/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147680153","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Application of accuracy profile-based evaluation in the development of quantitative methods for urinary phenol detection].","authors":"Xiao-Ning Liu, Yuan-Heng Shen, Wei-Feng Tang, Jun-Jie Ao, Jun-Xia Liu, Li Zhao, Li-Li Yuan, Xian Huang, Qian-Long Zhang","doi":"10.3724/SP.J.1123.2025.04031","DOIUrl":"10.3724/SP.J.1123.2025.04031","url":null,"abstract":"<p><p>Accurate and reliable analytical methods are fundamental to ensuring the validity and reproducibility of scientific results， particularly in research involving trace-level contaminants in biological samples. While standardized methods regulated by official guidelines are commonly used in certified laboratories， research laboratories often rely on in-house or self-developed non-standard methods tailored for specific studies. These methods， however， frequently lack harmonized validation criteria， especially regarding accuracy evaluation. Traditionally， method accuracy is assessed through single performance indicators such as recovery， relative standard deviation （RSD）， or bias. These indicators， although useful， may vary widely in their interpretation and offer limited insight into overall method performance， particularly when comparing between laboratories or over different concentration ranges. To address these limitations， the Société Française des Sciences et Techniques Pharmaceutiques （SFSTP） introduced the accuracy profile approach. This method integrates both trueness and precision using a statistical model to generate <i>β</i>-expectation tolerance intervals， allowing a visual and comprehensive representation of whether an analytical method meets predefined acceptance criteria across multiple concentration levels. Unlike traditional evaluations， which may obscure marginal performance failures， the accuracy profile provides a single， unified framework that simplifies interpretation and decision-making. In this study， we applied the SFSTP accuracy profile approach to validate a high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） method for quantifying 20 urinary phenols. Method performance was assessed at three concentration levels （low， medium， and high） and the results were compared with conventional validation methods. The intra-batch RSD values ranged from 2.8% to 10.7%， and inter-batch RSD values ranged from 3.3% to 14.4%. The pooled intermediate precision RSD ranged from 4.9% to 16.6%， indicating acceptable reproducibility. Relative errors were between -25.3% and 13.0%， According to traditional evaluation using single parameters， the accuracy of all 20 phenol measurements met standard criteria. However， accuracy profile analysis revealed that only 13 phenols， such as bisphenol AF and bisphenol B， had <i>β</i>-expectation tolerance intervals entirely within the ±30% acceptance limits across all tested concentration levels. The remaining seven phenols， including benzylparaben and benzophenone-8， exceeded acceptable limits at low or medium concentrations， suggesting areas for method optimization. In conclusion， this study demonstrates that the HPLC-MS/MS method provides reliable quantitative results for the majority of tested urinary phenols. More importantly， the SFSTP accuracy profile offers a superior alternative to conventional validation methods by combining accuracy parameters and risk analysis into a c","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"276-285"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980513/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147439020","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Determination of 30 homologues of phosphatidylcholines and lysophosphatidylcholines in human serum by liquid chromatography-tandem mass spectrometry and their correlation analysis with coronary artery disease].","authors":"Wen-Yu Li, Zhao-Yang Liu, Jun Dong, Rui-Yue Yang, Hong-Xia Li, Wen-Xiang Chen, Si-Ming Wang","doi":"10.3724/SP.J.1123.2025.08011","DOIUrl":"10.3724/SP.J.1123.2025.08011","url":null,"abstract":"<p><p>Phosphatidylcholine （PC） and lysophosphatidylcholine （LPC） homologues are closely associated with coronary atherosclerosis. Accurate determination of their contents can provide an important basis for the clinical diagnosis and prognosis of coronary artery disease （CAD）. In this study， an analytical method based on liquid chromatography-tandem mass spectrometry was established， which enabled the simultaneous and accurate determination of 30 PC and LPC homologues using only 10 μL of human serum. Methanol-acetonitrile-methyl <i>tert</i>-butyl methyl ether-water was used as the extraction system， and an XBridge C18 column was selected as the stationary phase. The mobile phase consisted of an acetonitrile-water mixture （1∶1， volume ratio） and isopropanol， both containing 7.5 mmol/L ammonium formate and 0.15% （volume ratio） formic acid， and gradient elution was adopted for separation. Detection was performed using an electrospray ionization source in the positive ion mode with multiple reaction monitoring. Method validation results showed that the method exhibited a good linear relationship， with an average linear correlation coefficient of ≥0.999 7 over a linear range of 0.125-100 μg/mL. The limits of detection and limits of quantification were 0.01-1.94 μg/mL and 0.03-6.48 μg/mL， respectively. The recoveries ranged from 85.4% to 114.3%， while the intra-day precision and inter-day precision were no more than 4.6% and 12.6%， respectively. Serum samples from 110 clinical volunteers who underwent coronary angiography were determined using this method. The average population concentration of PC homologues was 526.80 μg/mL， and that of LPC homologues was 73.67 μg/mL. Spearman correlation analysis revealed that PC and LPC homologues were closely correlated with the severity of CAD， as well as with related clinical biochemical and lipid metabolism indicators， suggesting that they could serve as potential CAD-related metabolites in clinical practice. Designed to meet clinical analysis needs， this method features small serum sample volume， simple operation， and excellent response. It can efficiently determine 30 PC and LPC homologues in human serum， providing an important reference for exploring the association between these two lipid classes and CAD， as well as the translational application of related biomarkers.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"234-247"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980518/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147439074","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Establishment and application of a knowledge-directed pseudo-targeted analytical method for diabetic retinopathy].","authors":"Yan-Qing Hou, Xiang-Yu Chi, Ting-Hu DU, Zeng-Qi Yan, Dai-di Hou, Chun-Xiu Hu, Yue-Xing Liu, Xin-Yu Liu, Guo-Wang Xu","doi":"10.3724/SP.J.1123.2025.02011","DOIUrl":"10.3724/SP.J.1123.2025.02011","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Diabetic retinopathy （DR） is a common blinding eye disease caused by diabetes mellitus and is the leading cause of acquired vision loss in adults worldwide. DR is asymptomatic in its early stages， and patients often miss the optimal treatment window by the time they seek medical attention due to vision impairment. Traditional methods used for DR diagnosis have inherent limitations and are not conducive to large-scale rapid screening. Biomarkers can reflect the stage of the disease owing to their specificity and sensitivity， which is crucial for the early diagnosis of DR. In the present study， 142 potential literature-based biomarkers associated with DR were included in a knowledge-directed strategy. And metabolites with different physicochemical properties were chromatographically separated using a 100-mm Discovery HS F5 column. A pseudo-targeted metabolomics method based on ultra-high performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS） that simultaneously scans positive and negative ions was established to improve analysis coverage and throughput. The method was validated using eight representative isotope-labeled internal standards as analytical targets. All isotope-labeled internal standards exhibited satisfactory linearities in both positive- and negative-ionization modes， with linear dynamic ranges spanning over three orders of magnitude and correlation coefficients （&lt;i&gt;r&lt;/i&gt;²） above 0.995. Extraction recoveries ranged between 75% and 108% at three distinct concentration levels with relative standard deviations （RSDs） below 13%. Notably， 91% of the isotope-labeled internal standards exhibited intra-day precision with RSDs of less than 5% across both ionization modes. Similarly， 91% of the analytes demonstrated inter-day precision with RSDs of less than 10%， with all below 16.3%， indicating good method precision. The developed method was used to analyze 137 serum samples， including 40 DR-free patients with diabetes mellitus （NDR） and 97 patients with DR to investigate the practicality of the method. Quality control （QC） samples were used to evaluate the data， which revealed that the instrument was stable during the analytical sequence. Partial least squares discriminant analysis （PLS-DA） models were constructed to identify and differentiate between the metabolic profiles of the DR and NDR groups with the aim of providing a statistical basis for the classification and diagnosis of DR based on metabolic differences observed in the serum samples. The NDR group and DR groups of varying clinical grades were well separated. A total of 85 differential metabolites were identified between NDR and DR groups using nonparametric tests. Further analysis led to the selection of choline and 12-hydroxyeicosatetraenoic acid （12-HETE） as two markers that effectively distinguished the DR and NDR groups. In addition， the markers exhibited a good ability to distinguish between DR and NDR patients when used in combination. The pseudo-tar","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"312-328"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980509/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147439097","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Performance validation and consistency assessment of three liquid chromatography-tandem mass spectrometry methods for detecting fat-soluble vitamins].","authors":"Bing-Chu Li, Bing-Hui Li, Zhi-Yang Chen, Zi-Yang Li, Mei-Ling Yin, Xing Lyu, Zhong-Yuan Xiang, Qi-Chen Long, Min Hu","doi":"10.3724/SP.J.1123.2025.04002","DOIUrl":"10.3724/SP.J.1123.2025.04002","url":null,"abstract":"<p><p>Accurate quantification of fat-soluble vitamin A （VA）， vitamin D （25（OH）D）， vitamin E （VE）， vitamin K （VK） is essential for health assessment and disease diagnosis. Liquid chromatography-tandem mass spectrometry （LC-MS/MS） plays a crucial role in the measurement of these vitamins due to its high specificity and sensitivity. However， the comparability and concordance of the detection results among different LC-MS/MS methods are still suboptimal. In this study， the analytical performance including linearity， limit of detection， limit of quantitation， precision， accuracy and carryover was evaluated according to CLSI C62 and <i>the Suggestions on Clinical Application of Liquid Chromatography-Mass Spectrometry</i>. Aliquots of 40 patient samples were collected from August to October 2022 from the Second Xiangya Hospital， Central South University. These fat-soluble vitamins were measured using three LC-MS/MS methods. Passing-Bablok regression， Bland-Altman plots and concordance correlation coefficient （CCC） were performed to compare the differences among three methods. The consistency of the results before and after recalibration with a unified calibrator was evaluated. The results showed that the total CVs for the three mass spectrometry kits were 2.7%-10.1%， and the recoveries for all kits ranged from 88.8% to 109.2%， indicating that their detection performance met the requirements for clinical application. Concordance correlation analysis showed that two of the three methods had substantial agreement in vitamin D testing （CCC： 0.938）， while the CCCs for other methods ranged from 0.322 to 0.853. After recalibration with a unified calibrator， except for vitamin K， the CCCs for the results of the three methods ranged from 0.918 to 0.983. In conclusion， the performance validation results of three LC-MS/MS methods for fat-soluble vitamins meet clinical requirements. The consistency among the three methods was poor， but using a unified calibrator significantly improved the consistency of these methods. The study provides recommendations for the standardization of clinical fat-soluble vitamin testing， thereby contributing to improved accuracy and consistency of results. This study will provide more reliable evidence for clinical diagnosis and treatment.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"267-275"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980508/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147439005","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Simultaneous determination of selinexor， posaconazole， venetoclax， and voriconazole in human plasma using ultra-high performance liquid chromatography-tandem mass spectrometry].","authors":"Xiong Xiao, Yue Li, Jin-Fang Hu, Qing Wan, Hong-Wei Peng","doi":"10.3724/SP.J.1123.2025.05003","DOIUrl":"10.3724/SP.J.1123.2025.05003","url":null,"abstract":"<p><p>Drugs used to treat hematologic malignancies often exhibit narrow therapeutic windows， significant inter-individual variability， and high risks of drug-drug interactions， necessitating therapeutic drug monitoring （TDM） for individualized dosing. For patients requiring concomitant antifungal therapy due to infections arising from severe chemotherapy-induced myelosuppression， TDM can optimize plasma concentrations of both antineoplastic and antifungal agents. This concurrent optimization ensures anti-tumor efficacy while effectively mitigating the risk of invasive fungal infections， positioning TDM as a critical component of personalized management in hematologic malignancies. This study established and validated a rapid ultra-high performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS） method for the simultaneous quantification of the antineoplastic agents selinexor （SEL） and venetoclax （VEN）， along with the antifungal agents voriconazole （VOR） and posaconazole （POSA） in human plasma. Chromatographic separation was achieved using a Kinetex^® XB-C18 column （50 mm × 3.0 mm， 2.6 µm） with a mobile phase consisting of methanol and 10 mmol/L ammonium acetate containing 0.1% formic acid， delivered at a flow rate of 0.5 mL/min under gradient elution conditions. The injection volume was 2 μL， and the total run time was 4.0 min. Detection employed an electrospray ionization source operating in positive ion mode with multiple reaction monitoring （MRM）. Following optimization of mass spectrometric parameters， the method underwent comprehensive validation. Calibration curves demonstrated excellent linearity （<i>r</i>>0.994） over the ranges of 0.04-1.48 μg/mL for SEL， 0.15-5.50 μg/mL for VEN， 0.29-11.77 μg/mL for VOR， and 0.15-6.05 μg/mL for POSA. Intra-day and inter-day precisions （RSDs） were ≤7.1% at all concentration levels. Extraction recoveries were ≥85.3%， demonstrating efficient and consistent sample processing. Method accuracy， determined by the percentage deviation of measured concentrations from nominal values， fell within the acceptable range of 87.4% to 109.0% across all QC levels， confirming the method's trueness. The practical utility of the validated UHPLC-MS/MS method was demonstrated through its application to clinical specimens. We collected and analyzed 81 clinical samples from 30 patients with acute myeloid leukemia treated with the combination of SEL and VEN. Measured plasma concentrations of SEL in these patients ranged from 0.049 μg/mL to 0.646 μg/mL. Notably， significant inter-individual variability in the peak plasma concentration （<i>C</i>_max） of SEL was observed within the same treatment cycle for approximately 30% of the patient cohort. This study offers evidence-based support for personalized precision therapy in this patient population， which exhibits substantial inter-individual variability and complex drug-drug interactions in clinical practice.</p>","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"349-356"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980512/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147438604","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Analysis of urine biomarkers in urothelial carcinoma based on untargeted metabolomics].","authors":"Sai Liu, Mo Wang, Wei Wang","doi":"10.3724/SP.J.1123.2025.05018","DOIUrl":"10.3724/SP.J.1123.2025.05018","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Urothelial carcinoma （UC） is a globally prevalent malignancy lacking robust non-invasive biomarkers. Metabolic reprogramming is a recognized cancer hallmark. Untargeted metabolomics enables high-throughput and unbiased analysis of bodily fluids， offering a promising approach for discovering novel biomarkers in UC. This investigation employs untargeted metabolomic profiling to detect novel urinary biomarkers in UC cohorts. The analytical strategy prioritizes tumor-associated metabolic perturbations through pathway-centric characterization of dysregulated biochemical networks. This study systematically characterizes differential metabolites and associated pathway dysregulations in UC cohorts. The approach seeks to establish a reliable metabolic signature with diagnostic and prognostic value. The findings are expected to advance the development of novel clinical tools. UC biomarkers should optimally integrate preclinical identification， treatment response tracking， and precision-tailored interventions. This investigation provides a methodological framework for exploring cancer metabolism in UC. And it offers evidence-based insights to support translational research and precision medicine initiatives in oncology. This study was conducted at Beijing Chao-Yang Hospital， Capital Medical University， between January and December 2020. A total of 60 urine specimens were consecutively collected. They comprised 30 histologically confirmed UC patients and 30 healthy controls with normal urinalysis findings. Clinical data was prospectively collected via structured case report forms. It encompassed baseline demographics， comorbidities， anthropometric and behavioral factors， and UC pathological parameters. All urine samples were collected prior to invasive procedures. And they were labeled， snap-frozen in liquid nitrogen， and stored at -80 ℃ until analysis. Metabolic profiling was performed using a quadrupole-orbitrap high resolution mass spectrometer equipped with a heated electrospray ionization source. Mass spectrometric data processing was performed using Progenesis QI software. Data processing followed the following workflow： raw data import， spectral peak alignment， feature extraction， and deconvolution. The Progenesis QI software generated datasets containing retention time， peak intensity， and mass-to-charge ratios. Multivariate signal decomposition enabled independent resolution of adduct species， including protonated and sodium-adducted ions. Quality control measures included elimination of ion features demonstrating intra-batch coefficient of variation &gt;15% across technical replicates. This rigorous preprocessing protocol ensured removal of unstable signals. And it preserved biologically relevant metabolic features for subsequent multivariate analysis. No statistically significant differences were observed in baseline clinical characteristics between UC and healthy control cohorts （&lt;i&gt;P&lt;/i&gt;&gt;0.05）. Untargeted metabolomic profiling was performed u","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"329-337"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980515/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147439065","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Application of chromatography-mass spectrometry in the clinical analysis of multiple sclerosis].","authors":"Zhen-Yu Yao, Yu-Fei Wang, Xiao-Wen Zhu, Hong Yang, Jia Wu, Guo-Jun Zhang","doi":"10.3724/SP.J.1123.2025.03024","DOIUrl":"10.3724/SP.J.1123.2025.03024","url":null,"abstract":"&lt;p&gt;&lt;p&gt;Multiple sclerosis （MuS） is a chronic， inflammatory， demyelinating disease of the central nervous system， with a globally increasing prevalence. Its pathogenesis involves complex interactions among immune dysregulation， genetic predisposition， and environmental factors. These contribute to a wide spectrum of clinical manifestations， posing significant challenges for both diagnosis and treatment. Metabolomics， the comprehensive analysis of small-molecule metabolites， has emerged as a powerful approach to elucidate MuS pathophysiology and identify potential biomarkers. In particular， alterations in amino acid and lipid metabolism are closely associated with inflammation， myelin damage， neurotransmitter imbalance， and immune activation. This review summarizes recent advancements in the application of chromatography-mass spectrometry techniques to MuS biomarker research. Key technologies include liquid chromatography-tandem mass spectrometry （LC-MS/MS） for analyzing metabolites in biological fluids， high resolution mass spectrometry （HRMS） for precise metabolite identification， gas chromatography-mass spectrometry （GC-MS） for profiling volatile compounds， and matrix-assisted laser desorption ionization-time of flight mass spectrometry （MALDI-TOF MS） for mapping spatial metabolite distributions in tissues. Metabolomic analyses of MuS patient samples have revealed significant disruptions in amino acid metabolism. For instance， reduced arginine levels and elevated asymmetric dimethylarginine levels in cerebrospinal fluid suggest vascular dysfunction. Altered tryptophan metabolism， including altered levels of kynurenic acid and 5-hydroxytryptophan， reflects neurotransmitter imbalances. Increased pyroglutamic acid levels indicate oxidative stress. Lipid metabolism is also markedly perturbed in MuS. Changes in palmitic acid levels affect cell membrane integrity， while alterations in sphingolipids， key components of myelin， are linked to demyelination. Elevated oxysterols correlate with neuroinflammation and immune dysregulation. Additionally， systemic lipid changes， such as reduced low-density lipoprotein and altered high-density lipoprotein cholesterol levels， have been associated with disease activity and progression. Due to their high sensitivity， resolution， and throughput， chromatography-mass spectrometry techniques are well-suited for detecting these metabolic alterations. Representative studies demonstrate the utility of LC-MS/MS in detecting amino acid perturbations in plasma and cerebrospinal fluid （CSF）， GC-MS in identifying lipid abnormalities in serum， HRMS in generating detailed brain tissue metabolite profiles， and MALDI-TOF MS in visualizing lesion-specific metabolic distributions. These findings have led to the identification of promising biomarker candidates. For instance， decreased arginine may indicate endothelial dysfunction， while elevated oxysterols may serve as markers of neuroinflammatory activity. Such biomarkers hold potenti","PeriodicalId":101336,"journal":{"name":"Se pu = Chinese journal of chromatography","volume":"44 3","pages":"226-233"},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12980507/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147439089","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}