Abstract Objective Currently, there is a significant gap in research on the processing methods for Artemisia rupestris L (YZH) in Xinjiang. This study systematically optimized the processing methods for A. rupestris L., using the content of its major active component, rupestonic acid, as an indicator, to increase the content of active ingredients and further advance research on the processing of YZH. Methods Through process optimization, this study identified the optimal preparation methods for YZH wine-processed, vinegar-processed, honey-processed, and ginger-processed. Subsequently, whole-spectrum metabolomics analysis was conducted to compare changes in the relative content of major active components, represented by rupestonic acid, under the optimal preparation methods. Finally, quantitative analysis of rupestonic acid was performed. Results Under the optimal processing methods of wine-processed, vinegar-processed, honey-processed, and ginger-processed YZH, compared to the raw material (2.92 mg g −1 ), the content of rupestonic acid in ginger-processed YZH (5.13 mg g −1 ) showed the most significant increase, approximately 75.7%, followed by vinegar-processed (4.02 mg g −1 , 38.4%) and wine-processed (3.85 mg g −1 , 31.8%). The rupestonic acid content in honey-processed YZH remained essentially unchanged. Full-spectrum metabolomics results showed that the levels of other major active components in ginger-processed YZH, such as chrysosplenetin, isovitexin, and rupestonic acid, also increased significantly. Conclusion Ginger, vinegar, and wine processing increase the content of active components in YZH, with ginger processing best preserving major active components represented by rupestonic acid. Ginger juice plays a central role in the ginger-processed preparation. While enhancing the therapeutic efficacy of YZH, it mitigates its bitter and cold nature, thereby reducing side effects on the human body, making it superior to traditional processing methods for raw herbal materials. Further research on this processing method is warranted in the future.
{"title":"Qualitative and quantitative analysis of the chemical constituents in different processed forms of Artemisia rupestris L","authors":"Hailong Song, He Cui","doi":"10.1556/1326.2026.01524","DOIUrl":"https://doi.org/10.1556/1326.2026.01524","url":null,"abstract":"Abstract Objective Currently, there is a significant gap in research on the processing methods for Artemisia rupestris L (YZH) in Xinjiang. This study systematically optimized the processing methods for A. rupestris L., using the content of its major active component, rupestonic acid, as an indicator, to increase the content of active ingredients and further advance research on the processing of YZH. Methods Through process optimization, this study identified the optimal preparation methods for YZH wine-processed, vinegar-processed, honey-processed, and ginger-processed. Subsequently, whole-spectrum metabolomics analysis was conducted to compare changes in the relative content of major active components, represented by rupestonic acid, under the optimal preparation methods. Finally, quantitative analysis of rupestonic acid was performed. Results Under the optimal processing methods of wine-processed, vinegar-processed, honey-processed, and ginger-processed YZH, compared to the raw material (2.92 mg g −1 ), the content of rupestonic acid in ginger-processed YZH (5.13 mg g −1 ) showed the most significant increase, approximately 75.7%, followed by vinegar-processed (4.02 mg g −1 , 38.4%) and wine-processed (3.85 mg g −1 , 31.8%). The rupestonic acid content in honey-processed YZH remained essentially unchanged. Full-spectrum metabolomics results showed that the levels of other major active components in ginger-processed YZH, such as chrysosplenetin, isovitexin, and rupestonic acid, also increased significantly. Conclusion Ginger, vinegar, and wine processing increase the content of active components in YZH, with ginger processing best preserving major active components represented by rupestonic acid. Ginger juice plays a central role in the ginger-processed preparation. While enhancing the therapeutic efficacy of YZH, it mitigates its bitter and cold nature, thereby reducing side effects on the human body, making it superior to traditional processing methods for raw herbal materials. Further research on this processing method is warranted in the future.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2026-08-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148861236","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract The binding interaction between arginine-poly(ester amide) (Arg-PEA), a novel polymeric carrier material, and RNA was investigated using capillary electrophoresis. The peak areas of free RNA molecules were analyzed after the interaction of RNA with various concentrations Arg-PEA in phosphate-buffered saline (pH 7.4) at different temperatures. The binding constant ( K A ) and number of binding sites ( n ) between Arg-PEA and RNA were calculated using the Lineweaver–Burk double reciprocal equation. Furthermore, by calculating the related thermodynamic parameters and performing computer-assisted molecular docking, the types of binding forces were investigated to confirm the mechanism of targeted binding. Results revealed that the unbound RNA molecules were effectively separated and detected by the capillary electrophoresis system. At 37 °C, the K A was 3.956 × 10 6 L·mol −1 and n was 2.48, indicating a powerful interaction between the two materials. The binding of Arg-PEA to RNA was primarily driven by electrostatic forces and supplemented by hydrogen bonding. These findings confirm the RNA-targeting efficacy of Arg-PEA used as a polymeric material for drug carrier construction. This study demonstrates capillary electrophoresis as a novel approach for studying the targeted binding of ligands to receptors, expanding the application scope of this technology.
{"title":"Investigation of the interaction between arginine-poly(ester amide) and RNA using capillary electrophoresis","authors":"Rui Xie, Chen Sun, Fengzhi Zhou, Yu Chen, Rong Xie, Yuqi Sun, Jianjun Zhang","doi":"10.1556/1326.2025.01383","DOIUrl":"https://doi.org/10.1556/1326.2025.01383","url":null,"abstract":"Abstract The binding interaction between arginine-poly(ester amide) (Arg-PEA), a novel polymeric carrier material, and RNA was investigated using capillary electrophoresis. The peak areas of free RNA molecules were analyzed after the interaction of RNA with various concentrations Arg-PEA in phosphate-buffered saline (pH 7.4) at different temperatures. The binding constant ( K A ) and number of binding sites ( n ) between Arg-PEA and RNA were calculated using the Lineweaver–Burk double reciprocal equation. Furthermore, by calculating the related thermodynamic parameters and performing computer-assisted molecular docking, the types of binding forces were investigated to confirm the mechanism of targeted binding. Results revealed that the unbound RNA molecules were effectively separated and detected by the capillary electrophoresis system. At 37 °C, the K A was 3.956 × 10 6 L·mol −1 and n was 2.48, indicating a powerful interaction between the two materials. The binding of Arg-PEA to RNA was primarily driven by electrostatic forces and supplemented by hydrogen bonding. These findings confirm the RNA-targeting efficacy of Arg-PEA used as a polymeric material for drug carrier construction. This study demonstrates capillary electrophoresis as a novel approach for studying the targeted binding of ligands to receptors, expanding the application scope of this technology.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"38 1","pages":"195-202"},"PeriodicalIF":0.0,"publicationDate":"2025-10-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147330996","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Citri Reticulatae Pericarpium (Chachi and Common mandarin), a dual-purpose traditional Chinese medicine (TCM) and food, contains bioactive flavonoids such as hesperidin, nobiletin, and tangeretin, which exhibit antioxidant, anti-inflammatory, and cardioprotective properties. However, conventional high-performance liquid chromatography with ultraviolet detection methods for their quantification are time-consuming (>80 min), environmentally unsustainable (high organic solvent use), and lack sensitivity for low-abundance components (e.g., nobiletin, tangeretin). To overcome these limitations, this study developed a rapid, eco-friendly method by integrating vortex-assisted matrix solid-phase dispersion with Poroshell column and high-performance liquid chromatography-mass spectrometry (HPLC-MS), reducing analysis time to 4 min (1 min extraction + 3 min HPLC-MS) and cutting solvent consumption by 75%. The optimized protocol demonstrated highly sensitive and efficient enabling precise quantification of target flavonoids in 24 batches Citri Reticulatae Pericarpium (12 batches each of Chachi and Common mandarin). The contents of hesperidin, nobiletin, and tangeretin in 24 batches of samples were 28.18–78.56, 0.24–3.30, and 0.11–2.80 mg g −1 dry weight, respectively. Finally, the greenness of the developed method was evaluated using the green analytical procedure index, which indicated a superior environmental profile with five green regions. Additionally, the blue applicability grade index tool was employed, resulting in a score of 80, reflecting high applicability and environmental friendliness. Results validated the method's robustness for rapid quality assessment of Citri Reticulatae Pericarpium, supporting TCM standardization and clinical safety. This advancement aligns with green analytical chemistry principles and offers a transformative approach for ultra-fast, sustainable herbal analysis.
摘要柑桔皮（chri Reticulatae Pericarpium, Chachi and Common mandarin）是一种双重用途的中药和食品，含有橙皮苷、褐皮素和橘皮素等生物活性黄酮类化合物，具有抗氧化、抗炎和保护心脏的作用。然而，传统的高效液相色谱紫外检测方法用于其定量是耗时（>；80分钟），环境不可持续（高有机溶剂的使用），并且对低丰度成分（如诺比列素，橘皮素）缺乏灵敏度。为了克服这些限制，本研究开发了一种快速、环保的方法，通过将涡流辅助基质固相分散与Poroshell柱和高效液相色谱-质谱（HPLC-MS）相结合，将分析时间缩短至4分钟（1分钟萃取+ 3分钟HPLC-MS），并将溶剂消耗减少75%。优化后的方案具有较高的灵敏度和效率，可对24批柑桔果皮（茶柑和普通柑各12批）中目标黄酮类化合物进行精确定量。24批样品中橙皮苷、褐皮苷和橘皮苷的含量分别为28.18 ~ 78.56、0.24 ~ 3.30和0.11 ~ 2.80 mg g−1干重。最后，利用绿色分析程序指数对该方法的绿色度进行了评价，结果表明该方法具有5个绿色区域的优越环境剖面。此外，采用蓝色适用性等级指标工具，得分为80分，反映了较高的适用性和环境友好性。结果验证了该方法对柑桔皮快速质量评价的稳健性，为中药标准化和临床安全性提供了依据。这一进步与绿色分析化学原理一致，为超快速、可持续的草药分析提供了一种变革性的方法。
{"title":"Minutes to measure: Ultra-fast and green HPLC-MS for flavonoid profiling in Citri Reticulatae Pericarpium","authors":"Jiabi Liang, Qinggui Lei, Guodong Chen, Wenhao Wang, Weiqi Yang, Zhengming Qian","doi":"10.1556/1326.2025.01366","DOIUrl":"https://doi.org/10.1556/1326.2025.01366","url":null,"abstract":"Abstract Citri Reticulatae Pericarpium (Chachi and Common mandarin), a dual-purpose traditional Chinese medicine (TCM) and food, contains bioactive flavonoids such as hesperidin, nobiletin, and tangeretin, which exhibit antioxidant, anti-inflammatory, and cardioprotective properties. However, conventional high-performance liquid chromatography with ultraviolet detection methods for their quantification are time-consuming (>80 min), environmentally unsustainable (high organic solvent use), and lack sensitivity for low-abundance components (e.g., nobiletin, tangeretin). To overcome these limitations, this study developed a rapid, eco-friendly method by integrating vortex-assisted matrix solid-phase dispersion with Poroshell column and high-performance liquid chromatography-mass spectrometry (HPLC-MS), reducing analysis time to 4 min (1 min extraction + 3 min HPLC-MS) and cutting solvent consumption by 75%. The optimized protocol demonstrated highly sensitive and efficient enabling precise quantification of target flavonoids in 24 batches Citri Reticulatae Pericarpium (12 batches each of Chachi and Common mandarin). The contents of hesperidin, nobiletin, and tangeretin in 24 batches of samples were 28.18–78.56, 0.24–3.30, and 0.11–2.80 mg g −1 dry weight, respectively. Finally, the greenness of the developed method was evaluated using the green analytical procedure index, which indicated a superior environmental profile with five green regions. Additionally, the blue applicability grade index tool was employed, resulting in a score of 80, reflecting high applicability and environmental friendliness. Results validated the method's robustness for rapid quality assessment of Citri Reticulatae Pericarpium, supporting TCM standardization and clinical safety. This advancement aligns with green analytical chemistry principles and offers a transformative approach for ultra-fast, sustainable herbal analysis.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-09-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147902695","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Ricolinostat (ACY-1215), a selective Histone Deacetylase 6 (HDAC6) inhibitor, exhibits potent antitumor activity against a broad spectrum of tumors. UPLC-MS/MS technique was employed to identify ACY-1215 in mouse plasma and investigate its pharmacokinetic variations following oral (10 and 30 mg kg −1 ) and intravenous (5 mg kg −1 ) administration. Protein precipitation method utilizing acetonitrile as the solvent and cilostazol as the internal standard (IS) was used for plasma preparation. Chromatographic separation was achieved using an UPLC High Strength Silica (HSS) T3 column with gradient elution employing acetonitrile and 0.1% formic acid in water mobile phase. The linear range of the ACY-1215 standard curve spanned from 0.5 to 1,000 ng mL −1 , exhibiting excellent linearity. Intra-day and inter-day precision were both below 10%, while accuracy ranged from 90 to 108%. Matrix effect fell within the range of 104 to 108%, with recovery exceeding 92%. The bioavailability of ACY-1215 was determined to be 54.4 and 48.4% after oral administration at doses of 10 and 30 mg kg −1 , respectively. The pharmacokinetics of ACY-1215 were successfully evaluated using the UPLC-MS/MS method.
Ricolinostat （acy1215）是一种选择性组蛋白去乙酰化酶6 （HDAC6）抑制剂，对多种肿瘤具有有效的抗肿瘤活性。采用UPLC-MS/MS技术鉴定小鼠血浆中的ACY-1215，并研究其口服（10和30 mg kg -1）和静脉（5 mg kg -1）给药后的药代动力学变化。血浆制备采用蛋白质沉淀法，以乙腈为溶剂，西洛他唑为内标（IS）。采用UPLC高强度二氧化硅（HSS） T3柱进行色谱分离，以乙腈和0.1%甲酸为水流动相进行梯度洗脱。ACY-1215标准曲线的线性范围为0.5 ~ 1,000 ng mL−1，具有良好的线性关系。日内和日间精度均低于10%，而精度在90 - 108%之间。基质效应在104 ~ 108%范围内，回收率超过92%。经测定，口服10 mg kg -1和30 mg kg -1后，ACY-1215的生物利用度分别为54.4%和48.4%。采用UPLC-MS/MS方法对ACY-1215的药动学进行了评价。
{"title":"Pharmacokinetics and bioavailability of ricolinostat in mouse plasma by UPLC-MS/MS","authors":"Lijing Zhang, Xicheng Dong, Jingsong Chi, Yishun Fan, Xiaohan Xin, Fangmei Zhang, Xianqin Wang, Jianshe Ma, Lulu Zhang","doi":"10.1556/1326.2025.01356","DOIUrl":"https://doi.org/10.1556/1326.2025.01356","url":null,"abstract":"Abstract Ricolinostat (ACY-1215), a selective Histone Deacetylase 6 (HDAC6) inhibitor, exhibits potent antitumor activity against a broad spectrum of tumors. UPLC-MS/MS technique was employed to identify ACY-1215 in mouse plasma and investigate its pharmacokinetic variations following oral (10 and 30 mg kg −1 ) and intravenous (5 mg kg −1 ) administration. Protein precipitation method utilizing acetonitrile as the solvent and cilostazol as the internal standard (IS) was used for plasma preparation. Chromatographic separation was achieved using an UPLC High Strength Silica (HSS) T3 column with gradient elution employing acetonitrile and 0.1% formic acid in water mobile phase. The linear range of the ACY-1215 standard curve spanned from 0.5 to 1,000 ng mL −1 , exhibiting excellent linearity. Intra-day and inter-day precision were both below 10%, while accuracy ranged from 90 to 108%. Matrix effect fell within the range of 104 to 108%, with recovery exceeding 92%. The bioavailability of ACY-1215 was determined to be 54.4 and 48.4% after oral administration at doses of 10 and 30 mg kg −1 , respectively. The pharmacokinetics of ACY-1215 were successfully evaluated using the UPLC-MS/MS method.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-08-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147897030","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Objectives This study aimed to explore the effective compounds and pharmacological mechanisms of Dendrobium officinale for the treatment of T2DM. Methods A qualitative analysis of effective compounds of D. officinale was performed by UPLC-ESI-Q-Orbitrap, network pharmacology analysis was used to preliminarily predict anti-T2DM mechanisms of D. officinale , virtual screening of effective compounds of D. officinale and validation of core protein targets were subsequently implemented through molecular docking technique. 3T3-L1 mouse preadipocytes was to validate the anti-T2DM therapeutic effect and pharmacological mechanism of D. officinale , relevant biochemical indexes and proteins were detected by biochemical assay kits and western blot method. Results There were 27 chemical compounds identified in D. officinale , anti-T2DM compounds of D. officinale were α-linolenic acid, naringenin, n-trans-feruloyltyramine, paprazine, et al. D. officinale extract could promote glucose uptake of 3T3-L1 cells in a dose-dependent manner and increase TG content in the cells, anti-T2DM mechanisms of D. officinale may involve PI3K/Akt, insulin resistance and insulin signaling pathways, core compounds of D. officinale were α-linolenic acid, naringenin, n-trans-feruloyltyramine, paprazine, isobutyl 4-hydroxybenzoate, pinellic acid, azelaic acid, acuminoside, rac-1-monopalmitoylglycerol and atractyloside A according to degree value of the network, anti-T2DM core targets of D. officinale were also screened out, including PIK3CA, AKT1, AKT2, MAPK1, MAPK3, MAP2K1, HRAS, PRKCA, MAPK8 and EGFR. Acuminoside, naringenin, n-trans-feruloyltyramine, et al. exhibited better affinity effects with PIK3CA, AKT1 and AKT2 while their docking scores were below −7.2 kcal mol −1 . The expressions of p-PI3K, p-AKT and GLUT4 in 3T3-L1 cells were significantly upregulated by D. officinale extract which indicated PI3K/Akt pathway was activated in insulin resistance and insulin signaling pathways of 3T3-L1 adipocytes under the therapeutic effect of D. officinale . Conclusions D. officinale could improve insulin resistance in T2DM by modulating PI3K/Akt, insulin resistance and insulin signaling pathways, acuminoside, naringenin, n-trans-feruloyltyramine, et al. from D. officinale could be used as anti-T2DM lead compounds with PI3K, AKT and GLUT4 as protein targets.
{"title":"Anti-type 2 diabetes mellitus compounds and pharmacological mechanism of Dendrobium officinale","authors":"Keyong Geng, Xiaoyan Zhang, Meiling Zeng, Bing Liang, Shilin Zhang, Yanqin Chen, Zhou We","doi":"10.1556/1326.2025.01347","DOIUrl":"https://doi.org/10.1556/1326.2025.01347","url":null,"abstract":"Abstract Objectives This study aimed to explore the effective compounds and pharmacological mechanisms of Dendrobium officinale for the treatment of T2DM. Methods A qualitative analysis of effective compounds of D. officinale was performed by UPLC-ESI-Q-Orbitrap, network pharmacology analysis was used to preliminarily predict anti-T2DM mechanisms of D. officinale , virtual screening of effective compounds of D. officinale and validation of core protein targets were subsequently implemented through molecular docking technique. 3T3-L1 mouse preadipocytes was to validate the anti-T2DM therapeutic effect and pharmacological mechanism of D. officinale , relevant biochemical indexes and proteins were detected by biochemical assay kits and western blot method. Results There were 27 chemical compounds identified in D. officinale , anti-T2DM compounds of D. officinale were α-linolenic acid, naringenin, n-trans-feruloyltyramine, paprazine, et al. D. officinale extract could promote glucose uptake of 3T3-L1 cells in a dose-dependent manner and increase TG content in the cells, anti-T2DM mechanisms of D. officinale may involve PI3K/Akt, insulin resistance and insulin signaling pathways, core compounds of D. officinale were α-linolenic acid, naringenin, n-trans-feruloyltyramine, paprazine, isobutyl 4-hydroxybenzoate, pinellic acid, azelaic acid, acuminoside, rac-1-monopalmitoylglycerol and atractyloside A according to degree value of the network, anti-T2DM core targets of D. officinale were also screened out, including PIK3CA, AKT1, AKT2, MAPK1, MAPK3, MAP2K1, HRAS, PRKCA, MAPK8 and EGFR. Acuminoside, naringenin, n-trans-feruloyltyramine, et al. exhibited better affinity effects with PIK3CA, AKT1 and AKT2 while their docking scores were below −7.2 kcal mol −1 . The expressions of p-PI3K, p-AKT and GLUT4 in 3T3-L1 cells were significantly upregulated by D. officinale extract which indicated PI3K/Akt pathway was activated in insulin resistance and insulin signaling pathways of 3T3-L1 adipocytes under the therapeutic effect of D. officinale . Conclusions D. officinale could improve insulin resistance in T2DM by modulating PI3K/Akt, insulin resistance and insulin signaling pathways, acuminoside, naringenin, n-trans-feruloyltyramine, et al. from D. officinale could be used as anti-T2DM lead compounds with PI3K, AKT and GLUT4 as protein targets.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2025-06-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://akjournals.com/downloadpdf/view/journals/1326/aop/article-10.1556-1326.2025.01347/article-10.1556-1326.2025.01347.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147919101","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Zhen Wang, Yanjun Gao, Xiaoru Ma, J L Zhang, Chenmiao Han, Zhijie Zhao, Weishuo Song, Rui-Ting Gu, Shijin Bu
Abstract An analytical method based on ion-pair liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed to accurately determine neomycin B in bovine edible tissues (muscle, kidney, liver, fat) and milk. The pre-treatment procedure, including protein precipitation and solid phase extraction, was investigated to extract the analytes of interest better and remove matrix interferences. After sample pre-treatment, the 1% heptafluorobutyric acid 20 μL was added to the final extract. Then, the chromatography and mass spectrometry conditions were optimized, and the established method was validated. Good linearity ( r > 0.999) was obtained at five matrices. The limit of detection, and the limit of quantitation were 10 and 20 μg kg −1 , respectively. Trueness and repeatability at 0.5× maximum residue limit (MRL), MRL, and 2× MRL ranged from 96.67 to 109.54% and 3.36 to 9.01%, respectively. Adding the ion-pair agent to the extracts, rather than the mobile phase, ensures that neomycin B is efficiently retained on the reverse-phase column without contaminating the ion source. This simple and sensitive LC-MS/MS method is suitable for regularly monitoring neomycin residue in bovine edible tissues and milk.
{"title":"Determination of neomycin B residue in bovine edible tissues and milk by ion-pair liquid chromatography-tandem mass spectrometry","authors":"Zhen Wang, Yanjun Gao, Xiaoru Ma, J L Zhang, Chenmiao Han, Zhijie Zhao, Weishuo Song, Rui-Ting Gu, Shijin Bu","doi":"10.1556/1326.2025.01283","DOIUrl":"https://doi.org/10.1556/1326.2025.01283","url":null,"abstract":"Abstract An analytical method based on ion-pair liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed to accurately determine neomycin B in bovine edible tissues (muscle, kidney, liver, fat) and milk. The pre-treatment procedure, including protein precipitation and solid phase extraction, was investigated to extract the analytes of interest better and remove matrix interferences. After sample pre-treatment, the 1% heptafluorobutyric acid 20 μL was added to the final extract. Then, the chromatography and mass spectrometry conditions were optimized, and the established method was validated. Good linearity ( r > 0.999) was obtained at five matrices. The limit of detection, and the limit of quantitation were 10 and 20 μg kg −1 , respectively. Trueness and repeatability at 0.5× maximum residue limit (MRL), MRL, and 2× MRL ranged from 96.67 to 109.54% and 3.36 to 9.01%, respectively. Adding the ion-pair agent to the extracts, rather than the mobile phase, ensures that neomycin B is efficiently retained on the reverse-phase column without contaminating the ion source. This simple and sensitive LC-MS/MS method is suitable for regularly monitoring neomycin residue in bovine edible tissues and milk.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"38 1","pages":"39-47"},"PeriodicalIF":0.0,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147903497","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Tea's beneficial effects have long been attributed to its abundance of natural bioactive compounds; however, the influence of variations in these compounds on taste and aroma remains poorly understood. To investigate the relationship between metabolomic profiles and tea processing adaptability, this study employed sensory evaluation and untargeted metabolomics to compare four tea cultivars from Guangxi—Ying Hong No.9 (YH), Gui Hong No.3 (GH), Gui Cha No.2 (GC), and Mei Zhan (MZ)—cultivated under the same conditions. Sensory evaluation revealed that GH and MZ exhibited the highest quality in green tea and black tea, respectively, while GC showed moderate quality, and YH performed less favorably than the other three cultivars. Metabolomics analysis uncovered significant differences in the metabolic profiles among the four tea cultivars, with MZ and YH displaying higher levels of flavonol glycosides, and GC and GH showing elevated levels of organic acids and fatty acids. Pathway analyses of GH and MZ indicated that the differentially enriched pathways were primarily related to linoleic acid metabolism and flavonoid and flavanol synthesis. Correlation analyses further revealed that the sensory quality of green tea was closely linked to fatty acids and organic acids in fresh leaves, whereas the sensory quality of black tea was strongly associated with flavonol glycoside levels. This study provides a comprehensive understanding of the complex relationship between metabolite characteristics and processing suitability in different tea cultivars, offering valuable insights into the development of tea germplasm resources in the Guangxi region.
{"title":"In-depth exploration of the correlation between metabolomic profiles and sensory attributes in Guangxi tea cultivars via LC-QTOF/MS analysis","authors":"Jing Wang, Yong Li, Huahong Liu, Zhusheng Liu, Yingyi Huang, Yuelan Pang, Wei Liuhua, Yun Zhang, Jinfang Nie","doi":"10.1556/1326.2024.01295","DOIUrl":"https://doi.org/10.1556/1326.2024.01295","url":null,"abstract":"Abstract Tea's beneficial effects have long been attributed to its abundance of natural bioactive compounds; however, the influence of variations in these compounds on taste and aroma remains poorly understood. To investigate the relationship between metabolomic profiles and tea processing adaptability, this study employed sensory evaluation and untargeted metabolomics to compare four tea cultivars from Guangxi—Ying Hong No.9 (YH), Gui Hong No.3 (GH), Gui Cha No.2 (GC), and Mei Zhan (MZ)—cultivated under the same conditions. Sensory evaluation revealed that GH and MZ exhibited the highest quality in green tea and black tea, respectively, while GC showed moderate quality, and YH performed less favorably than the other three cultivars. Metabolomics analysis uncovered significant differences in the metabolic profiles among the four tea cultivars, with MZ and YH displaying higher levels of flavonol glycosides, and GC and GH showing elevated levels of organic acids and fatty acids. Pathway analyses of GH and MZ indicated that the differentially enriched pathways were primarily related to linoleic acid metabolism and flavonoid and flavanol synthesis. Correlation analyses further revealed that the sensory quality of green tea was closely linked to fatty acids and organic acids in fresh leaves, whereas the sensory quality of black tea was strongly associated with flavonol glycoside levels. This study provides a comprehensive understanding of the complex relationship between metabolite characteristics and processing suitability in different tea cultivars, offering valuable insights into the development of tea germplasm resources in the Guangxi region.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-12-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147900263","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Eleutherococcus senticosus (Rupr. & Maxim.) Maxim. fruits (ESF) is a natural health food that has been widely used in traditional medicine. This study aimed to establish and validate a rapid and sensitive method for determining of six phenolic acids in plasma of normal and T2DM rats by ultra-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). Separation and quantification were performed on a Waters HSS T3 column (100 × 2.1 mm, 1.8 μm) with water (A) and methanol (B). The electrospray ionization (ESI) source was operated in negative ionization mode. Multiple reaction monitoring (MRM) was used to quantitatively analyzed hyperoside m / z 463.2→301.1, caffeic acid m / z 179.1→135.1, chlorogenic acid m / z 353.2→190.9, gallic acid m / z 169.0→125.1, protocatechuic acid m / z 153.1→109.1, and isofraxidin m / z 221.1→191.0, respectively. The hypoglycemic effect of ESF was verified by determining blood glucose and lipid levels in a type 2 diabetes model. This study laid the foundation for exploring ESF clinical guidelines in the future.
摘要：感刺棘球绦虫（Eleutherococcus senticosus）；和箴言)。的格言。水果是一种天然的保健食品，在传统医学中有着广泛的应用。本研究旨在建立一种快速、灵敏的超高效液相色谱-串联质谱（UHPLC-MS/MS）测定正常和2型糖尿病大鼠血浆中6种酚酸的方法。采用Waters HSS T3色谱柱（100 × 2.1 mm, 1.8 μm），水(a)和甲醇(B)进行分离和定量。电喷雾电离源工作在负电离模式下。采用多重反应监测（MRM）法，分别定量分析金丝桃苷m / z 463.2→301.1、咖啡酸m / z 179.1→135.1、绿原酸m / z 353.2→190.9、没食子酸m / z 169.0→125.1、原儿茶酸m / z 153.1→109.1、异黄皮苷m / z 221.1→191.0。通过测定2型糖尿病模型的血糖和血脂水平，证实了ESF的降糖作用。本研究为今后探索ESF临床指南奠定了基础。
{"title":"LC-MS/MS method for the simultaneous determination of six phenolic acids in rat plasma and hypoglycemic effects in normal and T2DM rats after oral administration of Eleutherococcus senticosus fruits extract","authors":"Jingnan Chen, Yanping Sun, Sen Li, Haibo Wu, Lijia Guo, Yuxin Wei, Yunwei Liu, Xiangquan Li, Meng Wang, Zhenyue Wang, Zhibin Wang","doi":"10.1556/1326.2024.01253","DOIUrl":"https://doi.org/10.1556/1326.2024.01253","url":null,"abstract":"Abstract Eleutherococcus senticosus (Rupr. & Maxim.) Maxim. fruits (ESF) is a natural health food that has been widely used in traditional medicine. This study aimed to establish and validate a rapid and sensitive method for determining of six phenolic acids in plasma of normal and T2DM rats by ultra-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). Separation and quantification were performed on a Waters HSS T3 column (100 × 2.1 mm, 1.8 μm) with water (A) and methanol (B). The electrospray ionization (ESI) source was operated in negative ionization mode. Multiple reaction monitoring (MRM) was used to quantitatively analyzed hyperoside m / z 463.2→301.1, caffeic acid m / z 179.1→135.1, chlorogenic acid m / z 353.2→190.9, gallic acid m / z 169.0→125.1, protocatechuic acid m / z 153.1→109.1, and isofraxidin m / z 221.1→191.0, respectively. The hypoglycemic effect of ESF was verified by determining blood glucose and lipid levels in a type 2 diabetes model. This study laid the foundation for exploring ESF clinical guidelines in the future.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"37 3","pages":"294-306"},"PeriodicalIF":0.0,"publicationDate":"2024-12-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147881757","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract SZJ-1207 is a natural product extracted from Stephanotis mucronata (Blanco) Merr which has significant antidepressant effects in various depression mouse models, without obvious acute toxicity or sedative-hypnotic side effects. The aim of this study was to preliminarily clarify the pharmacokinetic characteristics of SZJ-1207 in rats after a single intragastric and intravenous administration. In this study, sensitive and reliable UPLC-MS/MS quantification methods were established and then successfully applied to the pharmacokinetic study of SZJ-1207 in rats. The linear range of SZJ-1207 were 0.5–400 ng mL −1 in plasma, feaces, bile and 20–4,000 ng mL −1 in urine, respectively ( r > 0.99). All methods met the requirements of ICH M10. The results of pharmaconetic study showed that C max , AUC (0-t) and AUC (0-∞) had linear relationships with the administered doses in the range of 0.5–4.5 mg kg −1 . There was a significant gender difference in the AUC (0-t) of 0.5 and 1.5 mg kg −1 and C max of 1.5 mg kg −1 after ig ( P < 0.05). The excretion rates of SZJ-1207 were 8.46 ± 4.82% in feces, 1.89 ± 1.08% in urine, and 0.179 ± 0.118% in bile. The oral absolute bioavailability of SZJ-1207 was calculated as 64.64%.
摘要：SZJ-1207是一种天然提取物，在多种抑郁症小鼠模型中均有明显的抗抑郁作用，无明显的急性毒性和镇静催眠副作用。本研究的目的是初步阐明SZJ-1207单次灌胃和静脉给药后在大鼠体内的药代动力学特征。本研究建立了灵敏可靠的UPLC-MS/MS定量方法，并成功应用于SZJ-1207在大鼠体内的药动学研究。SZJ-1207在血浆、面部、胆汁和尿液中的线性范围分别为0.5 ~ 400 ng mL -1和20 ~ 4000 ng mL -1 （r > 0.99）。所有方法均符合ICH M10的要求。药效学研究结果表明，在0.5 ~ 4.5 mg kg - 1范围内，cmax、AUC （0-t）和AUC（0-∞）与给药剂量呈线性关系。ig后的AUC （0-t）为0.5和1.5 mg kg - 1， cmax为1.5 mg kg - 1，性别差异显著（P < 0.05）。SZJ-1207在粪便中的排泄率为8.46±4.82%，在尿液中的排泄率为1.89±1.08%，在胆汁中的排泄率为0.179±0.118%。计算出SZJ-1207的口服绝对生物利用度为64.64%。
{"title":"UPLC-MS/MS analysis of SZJ-1207 in rat plasma, urine, feces and bile for pharmacokinetic studies","authors":"Haiyang Lin, Yingying Sun, Bingying Hu, Jinjun Fang, Zhen Ge, Zhisheng He, Yang Wei","doi":"10.1556/1326.2024.01221","DOIUrl":"https://doi.org/10.1556/1326.2024.01221","url":null,"abstract":"Abstract SZJ-1207 is a natural product extracted from Stephanotis mucronata (Blanco) Merr which has significant antidepressant effects in various depression mouse models, without obvious acute toxicity or sedative-hypnotic side effects. The aim of this study was to preliminarily clarify the pharmacokinetic characteristics of SZJ-1207 in rats after a single intragastric and intravenous administration. In this study, sensitive and reliable UPLC-MS/MS quantification methods were established and then successfully applied to the pharmacokinetic study of SZJ-1207 in rats. The linear range of SZJ-1207 were 0.5–400 ng mL −1 in plasma, feaces, bile and 20–4,000 ng mL −1 in urine, respectively ( r > 0.99). All methods met the requirements of ICH M10. The results of pharmaconetic study showed that C max , AUC (0-t) and AUC (0-∞) had linear relationships with the administered doses in the range of 0.5–4.5 mg kg −1 . There was a significant gender difference in the AUC (0-t) of 0.5 and 1.5 mg kg −1 and C max of 1.5 mg kg −1 after ig ( P < 0.05). The excretion rates of SZJ-1207 were 8.46 ± 4.82% in feces, 1.89 ± 1.08% in urine, and 0.179 ± 0.118% in bile. The oral absolute bioavailability of SZJ-1207 was calculated as 64.64%.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"37 2","pages":"155-163"},"PeriodicalIF":0.0,"publicationDate":"2024-05-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147330440","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
This review focuses on monosodium glutamate which proclaims the fifth taste as “Umami”. Monosodium glutamate imparts a deep, meaty, umami flavour to foods. Asian cuisine frequently uses this flavouring, just as in the processed items produced across the United States and Europe. This article dealt with a detailed discussion of physicochemical features, pharmacological actions, and different reported analytical methodologies for the estimation of monosodium glutamate. Monosodium glutamate is analyzed using a variety of techniques, including spectroscopy, chromatography, electrochemistry, electrophoresis, chemometrics, flow injection analysis, and biosensors. According to results of comparative research of analytical methodologies, high performance liquid chromatography (HPLC) is most widely used method for analyzing monosodium glutamate which surpasses the gas chromatographic (GC) approach. All of the reported methods are accurate, precise, cost-effective, and sensitive. The European Union defined monosodium glutamate as a food additive that is permitted in some foods, but is subject to quantitative limits. Consequently, this study provides the analyst with an accessible path to quantifying monosodium glutamate's content for use in the food and pharmaceutical industries.
{"title":"A comprehensive assessment of the biological attributes of and analytical quantification methods for monosodium glutamate","authors":"Atyurmila Chakraborty, Kavitha Jayaseelan","doi":"10.1556/1326.2023.01171","DOIUrl":"https://doi.org/10.1556/1326.2023.01171","url":null,"abstract":"This review focuses on monosodium glutamate which proclaims the fifth taste as “Umami”. Monosodium glutamate imparts a deep, meaty, umami flavour to foods. Asian cuisine frequently uses this flavouring, just as in the processed items produced across the United States and Europe. This article dealt with a detailed discussion of physicochemical features, pharmacological actions, and different reported analytical methodologies for the estimation of monosodium glutamate. Monosodium glutamate is analyzed using a variety of techniques, including spectroscopy, chromatography, electrochemistry, electrophoresis, chemometrics, flow injection analysis, and biosensors. According to results of comparative research of analytical methodologies, high performance liquid chromatography (HPLC) is most widely used method for analyzing monosodium glutamate which surpasses the gas chromatographic (GC) approach. All of the reported methods are accurate, precise, cost-effective, and sensitive. The European Union defined monosodium glutamate as a food additive that is permitted in some foods, but is subject to quantitative limits. Consequently, this study provides the analyst with an accessible path to quantifying monosodium glutamate's content for use in the food and pharmaceutical industries.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"12 10","pages":""},"PeriodicalIF":1.9,"publicationDate":"2024-01-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139438697","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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