To investigate the mechanism of Radix Rehmanniae Praeparata (RRP) in treating blood deficiency syndrome (BDS) by analyzing the changes in chemical components before and after processing, and its effects on metabolomics and gut microbiota in BDS mice.
Methods
Ultra-high-performance liquid chromatographyquadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) was employed to screen differential components before and after the processing of Radix Rehmanniae (RR). Pharmacodynamic studies were conducted to validate the therapeutic effects. Additionally, UPLC-Q-TOF-MS, headspace sampling-gas chromatography-mass spectrometry (HS-GC-MS), and 16sRNA sequencing were used to investigate the regulatory effects of RRP on metabolomics and the gut microbiota in BDS mice.
Results
The primary differential components identified were iridoids, phenylethanoid glycosides, sugars, benzaldehydes, and 5-hydroxymethylfurfural and its derivatives. RRP effectively ameliorated blood and energy metabolism in BDS mice. It regulates the biosynthesis pathway of unsaturated fatty acids, increases the abundance of Firmicutes to elevate butyric acid levels, and reduces the abundance of Bacteroidetes to downregulate acetic and propionic acid levels, thereby exerting therapeutic effects on BDS.
Conclusion
RRP attenuated the metabolic state of BDS mice by modulating metabolic pathways and gut microbiota balance, providing a scientific basis for its clinical application.
{"title":"Mechanisms of radix rehmanniae praeparata in treating blood deficiency: A study on chemistry, metabolomics, and gut microbiota","authors":"RuXi GAO, FanYi WANG, Xiang LIU, Chu YUAN, GuoShun SHAN","doi":"10.1016/j.cjac.2025.100548","DOIUrl":"10.1016/j.cjac.2025.100548","url":null,"abstract":"<div><h3>Objective</h3><div>To investigate the mechanism of Radix Rehmanniae Praeparata (RRP) in treating blood deficiency syndrome (BDS) by analyzing the changes in chemical components before and after processing, and its effects on metabolomics and gut microbiota in BDS mice.</div></div><div><h3>Methods</h3><div>Ultra-high-performance liquid chromatographyquadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS) was employed to screen differential components before and after the processing of Radix Rehmanniae (RR). Pharmacodynamic studies were conducted to validate the therapeutic effects. Additionally, UPLC-Q-TOF-MS, headspace sampling-gas chromatography-mass spectrometry (HS-GC-MS), and 16sRNA sequencing were used to investigate the regulatory effects of RRP on metabolomics and the gut microbiota in BDS mice.</div></div><div><h3>Results</h3><div>The primary differential components identified were iridoids, phenylethanoid glycosides, sugars, benzaldehydes, and 5-hydroxymethylfurfural and its derivatives. RRP effectively ameliorated blood and energy metabolism in BDS mice. It regulates the biosynthesis pathway of unsaturated fatty acids, increases the abundance of Firmicutes to elevate butyric acid levels, and reduces the abundance of Bacteroidetes to downregulate acetic and propionic acid levels, thereby exerting therapeutic effects on BDS.</div></div><div><h3>Conclusion</h3><div>RRP attenuated the metabolic state of BDS mice by modulating metabolic pathways and gut microbiota balance, providing a scientific basis for its clinical application.</div></div>","PeriodicalId":277,"journal":{"name":"Chinese Journal of Analytical Chemistry","volume":"53 7","pages":"Article 100548"},"PeriodicalIF":1.2,"publicationDate":"2025-04-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144154812","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}
Pub Date : 2025-04-16DOI: 10.1016/j.cjac.2025.100551
Junying WU , Qiong AN , Zhenggen LIAO , Yulin FENG , Wuliang YANG , Haifang CHEN , Wugang ZHANG
Hyperuricemia arises from an imbalance between uric acid production and excretion, resulting in elevated systemic uric acid levels. Consequently, therapeutic strategies targeting both production and excretion pathways offer a promising approach for managing hyperuricemia. TongFengTangSan (TFTS) has been frequently utilized as the Tibetan prescription in treating hyperuricemia or gout, and its anti-hyperuricemia effect has been confirmed in our previous study. However, the urate-lowering components still remain unclear. Therefore, an integrative strategy was constructed to screen potential urate-lowering components from TFTS by combination with affinity ultrafiltration, molecular docking and in vitro validation. In the present study, the main active fraction of TFTS with xanthine oxidase inhibitory effect was screened out by xanthine oxidase inhibitory assay. The potential ligands in main active fraction were identified by affinity ultrafiltration experiment combined with enzyme channel blocking technology and explored by ultra-high performance liquid chromatography-linear ion trap-Orbitrap mass spectrometry. Then, the screened ligands were further validated by in vitro xanthine oxidase inhibitory assay and molecular docking technique. Furthermore, the regulation effect on uric acid transporters of xanthine oxidase inhibitors was further evaluated by the over-expression of uric acid transporters in uric acid stimulated human Kidney-2 cell model by Western blot assay. In this study, the 60% ethanol-eluted fraction from the ethanol extract of TFTS was confirmed as the main fraction of TFTS with the best xanthine oxidase inhibitory effect. Three potential xanthine oxidase inhibitors were screened out from the 60% ethanol-eluted fraction, including 1,3,6-trigalloylglucose, 1,2,3,6-tetragalloylglucose and 1,2,3,4,6-pentagalloylglucose. Half maximal inhibitory concentration values of 1,3,6-trigalloylglucose, 1,2,3,6-tetragalloylglucose and 1,2,3,4,6-pentagalloylglucose for xanthine oxidase were 54.46, 15.91, 6.58 μg/mL, respectively. 1,3,6-trigalloylglucose, 1,2,3,6-tetragalloylglucose and 1,2,3,4,6-pentagalloylglucose were identified as mixed-type xanthine oxidase inhibitors. Additionally, these compounds demonstrated inhibitory effects on urate transporters 1 and glucose transporter 9. The combination strategy is suitable for screening active components with dual properties of inhibiting uric acid production and promoting uric acid excretion. 1,3,6-trigalloylglucose, 1,2,3,6-tetragalloylglucose and 1,2,3,4,6-pentagalloylglucose were identified as a potential urate-lowering drug and exhibited dual-target characteristics in uric acid metabolism.
{"title":"Screening of urate-lowering components in TongFengTangSan using an integrated strategy of affinity ultrafiltration, molecular docking and in vitro validation","authors":"Junying WU , Qiong AN , Zhenggen LIAO , Yulin FENG , Wuliang YANG , Haifang CHEN , Wugang ZHANG","doi":"10.1016/j.cjac.2025.100551","DOIUrl":"10.1016/j.cjac.2025.100551","url":null,"abstract":"<div><div>Hyperuricemia arises from an imbalance between uric acid production and excretion, resulting in elevated systemic uric acid levels. Consequently, therapeutic strategies targeting both production and excretion pathways offer a promising approach for managing hyperuricemia. TongFengTangSan (TFTS) has been frequently utilized as the Tibetan prescription in treating hyperuricemia or gout, and its anti-hyperuricemia effect has been confirmed in our previous study. However, the urate-lowering components still remain unclear. Therefore, an integrative strategy was constructed to screen potential urate-lowering components from TFTS by combination with affinity ultrafiltration, molecular docking and <em>in vitro</em> validation. In the present study, the main active fraction of TFTS with xanthine oxidase inhibitory effect was screened out by xanthine oxidase inhibitory assay. The potential ligands in main active fraction were identified by affinity ultrafiltration experiment combined with enzyme channel blocking technology and explored by ultra-high performance liquid chromatography-linear ion trap-Orbitrap mass spectrometry. Then, the screened ligands were further validated by <em>in vitro</em> xanthine oxidase inhibitory assay and molecular docking technique. Furthermore, the regulation effect on uric acid transporters of xanthine oxidase inhibitors was further evaluated by the over-expression of uric acid transporters in uric acid stimulated human Kidney-2 cell model by Western blot assay. In this study, the 60% ethanol-eluted fraction from the ethanol extract of TFTS was confirmed as the main fraction of TFTS with the best xanthine oxidase inhibitory effect. Three potential xanthine oxidase inhibitors were screened out from the 60% ethanol-eluted fraction, including 1,3,6-trigalloylglucose, 1,2,3,6-tetragalloylglucose and 1,2,3,4,6-pentagalloylglucose. Half maximal inhibitory concentration values of 1,3,6-trigalloylglucose, 1,2,3,6-tetragalloylglucose and 1,2,3,4,6-pentagalloylglucose for xanthine oxidase were 54.46, 15.91, 6.58 μg/mL, respectively. 1,3,6-trigalloylglucose, 1,2,3,6-tetragalloylglucose and 1,2,3,4,6-pentagalloylglucose were identified as mixed-type xanthine oxidase inhibitors. Additionally, these compounds demonstrated inhibitory effects on urate transporters 1 and glucose transporter 9. The combination strategy is suitable for screening active components with dual properties of inhibiting uric acid production and promoting uric acid excretion. 1,3,6-trigalloylglucose, 1,2,3,6-tetragalloylglucose and 1,2,3,4,6-pentagalloylglucose were identified as a potential urate-lowering drug and exhibited dual-target characteristics in uric acid metabolism.</div></div>","PeriodicalId":277,"journal":{"name":"Chinese Journal of Analytical Chemistry","volume":"53 7","pages":"Article 100551"},"PeriodicalIF":1.2,"publicationDate":"2025-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144170000","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}
Pub Date : 2025-04-16DOI: 10.1016/j.cjac.2025.100547
Sha ZHANG , Kemeng CAO , Peipei ZHAO , Yuanyuan WANG , Qiuyue XU , Bin YUAN , Mingchen JIANG
Background
Respiratory syncytial virus (RSV) is one of the leading pathogens associated with hospitalization for childhood pneumonia and is associated with substantial morbidity and fatality among young children and infants. There are no specific antiviral treatments for RSV infections. Kaempferol, a flavonoid present in traditional Chinese medicines, possesses antiviral activity and may affect RSV-induced lung inflammation; however, this relationship remains unclear.
Methods
We employed network pharmacology to forecast the mechanism of kaempferol in the treatment of RSV pneumonia, and used gas chromatography-mass spectrometry (GC-MS) to examine the metabolic profiles in serum. We then integrated the analysis of differential metabolites with potential targets using MetScape and assessed the interactions between kaempferol and the key targets through molecular docking. Molecular biology experiments confirmed these predictions.
Results
Our results demonstrated that kaempferol alleviated RSV-induced lung inflammation, inhibited viral replication, and reduced lung damage, possibly by modulating the JAK-STAT signaling pathway. Kaempferol primarily alleviates metabolic disorders by targeting amino acid metabolism. Molecular docking analysis indicated a strong binding affinity of kaempferol for AKT1, CASP3, SRC, EGFR, STAT1, and IL-2.
Conclusion
Kaempferol ameliorated the metabolic disruptions caused by RSV in the amino acid metabolism, via the JAK-STAT signaling cascade and mitigated the inflammatory response associated with RSV infection. This study not only provides foundational data for the broad application of kaempferol in anti-RSV research but also offers novel insights into the exploration of therapeutic mechanisms for RSV infections.
{"title":"Unveiling the mechanism of kaempferol in RSV-induced lung inflammation through metabolomics and network pharmacology","authors":"Sha ZHANG , Kemeng CAO , Peipei ZHAO , Yuanyuan WANG , Qiuyue XU , Bin YUAN , Mingchen JIANG","doi":"10.1016/j.cjac.2025.100547","DOIUrl":"10.1016/j.cjac.2025.100547","url":null,"abstract":"<div><h3>Background</h3><div>Respiratory syncytial virus (RSV) is one of the leading pathogens associated with hospitalization for childhood pneumonia and is associated with substantial morbidity and fatality among young children and infants. There are no specific antiviral treatments for RSV infections. Kaempferol, a flavonoid present in traditional Chinese medicines, possesses antiviral activity and may affect RSV-induced lung inflammation; however, this relationship remains unclear.</div></div><div><h3>Methods</h3><div>We employed network pharmacology to forecast the mechanism of kaempferol in the treatment of RSV pneumonia, and used gas chromatography-mass spectrometry (GC-MS) to examine the metabolic profiles in serum. We then integrated the analysis of differential metabolites with potential targets using MetScape and assessed the interactions between kaempferol and the key targets through molecular docking. Molecular biology experiments confirmed these predictions.</div></div><div><h3>Results</h3><div>Our results demonstrated that kaempferol alleviated RSV-induced lung inflammation, inhibited viral replication, and reduced lung damage, possibly by modulating the JAK-STAT signaling pathway. Kaempferol primarily alleviates metabolic disorders by targeting amino acid metabolism. Molecular docking analysis indicated a strong binding affinity of kaempferol for AKT1, CASP3, SRC, EGFR, STAT1, and IL-2.</div></div><div><h3>Conclusion</h3><div>Kaempferol ameliorated the metabolic disruptions caused by RSV in the amino acid metabolism, via the JAK-STAT signaling cascade and mitigated the inflammatory response associated with RSV infection. This study not only provides foundational data for the broad application of kaempferol in anti-RSV research but also offers novel insights into the exploration of therapeutic mechanisms for RSV infections.</div></div>","PeriodicalId":277,"journal":{"name":"Chinese Journal of Analytical Chemistry","volume":"53 7","pages":"Article 100547"},"PeriodicalIF":1.2,"publicationDate":"2025-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144108259","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}
Pub Date : 2025-04-16DOI: 10.1016/j.cjac.2025.100549
Genhua ZHU , Liji ZHONG , Yonggui SONG , Youhui ZHANG , Luting YAN , Zhifu AI , Ming YANG , Yali LIU , Yuhui PING , Huihui LIANG , Dan SU
Saponins, the primary bioactive components of Achyranthes bidentata Blume (AB), exhibit neuroprotective and anti-inflammatory properties. However, the lack of pharmacokinetic (PK) data, particularly on tissue distribution and first-pass effects, critically hinders their therapeutic development. Therefore, a rapid ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) method (9-min run time) was validated to simultaneously quantify five AB saponins in mice tissues (brain, heart, liver, spleen, lung, kidney; n = 5 per time point) at 10, 30, 60, 120, 240 min post-administration. The method demonstrated excellent linearity (R2 > 0.99, 1–2500 ng/mL), precision (RSD ≤ 7.04 %), accuracy (85%–115 %), and recovery rates (86.6%–97.2 %, RSD ≤ 11.39 %) per ICH M10 guidelines. The results demonstrate that the saponin concentrations in various tissues after IG and IP administration were lower compared to those after IV administration, with levels reaching only 10 % of the latter. Although all these compounds are pentacyclic triterpenoid saponins with an oleanane skeleton, their tissue distribution in vivo varies significantly. The elimination of achyranthoside D, ginsenoside R0, and araloside A is relatively slow in various tissues. In contrast, chikusetsusaponin IVa is rapidly eliminated from various tissues. The ability of four saponins to cross the blood-brain barrier is highly beneficial for the development of therapeutic drugs for central nervous system diseases. Additionally, the results from different administration routes indicate that AB saponins may exhibit a pronounced gastrointestinal and hepatic first-pass effect in vivo, which should be considered in future research. This study can guide multi-route study of AB saponins provides critical insights for formulation optimization and dosing regimen design to mitigate first-pass effects
{"title":"Comparative tissue distribution analysis of Achyranthes bidentata Blume saponins via intragastric, intraperitoneal, and intravenous administration using simultaneous UPLC-MS/MS detection","authors":"Genhua ZHU , Liji ZHONG , Yonggui SONG , Youhui ZHANG , Luting YAN , Zhifu AI , Ming YANG , Yali LIU , Yuhui PING , Huihui LIANG , Dan SU","doi":"10.1016/j.cjac.2025.100549","DOIUrl":"10.1016/j.cjac.2025.100549","url":null,"abstract":"<div><div>Saponins, the primary bioactive components of <em>Achyranthes bidentata Blum</em>e (AB), exhibit neuroprotective and anti-inflammatory properties. However, the lack of pharmacokinetic (PK) data, particularly on tissue distribution and first-pass effects, critically hinders their therapeutic development. Therefore, a rapid ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) method (9-min run time) was validated to simultaneously quantify five AB saponins in mice tissues (brain, heart, liver, spleen, lung, kidney; n = 5 per time point) at 10, 30, 60, 120, 240 min post-administration. The method demonstrated excellent linearity (<em>R</em><sup>2</sup> > 0.99, 1–2500 ng/mL), precision (RSD ≤ 7.04 %), accuracy (85%–115 %), and recovery rates (86.6%–97.2 %, RSD ≤ 11.39 %) per ICH M10 guidelines. The results demonstrate that the saponin concentrations in various tissues after IG and IP administration were lower compared to those after IV administration, with levels reaching only 10 % of the latter. Although all these compounds are pentacyclic triterpenoid saponins with an oleanane skeleton, their tissue distribution <em>in vivo</em> varies significantly. The elimination of achyranthoside D, ginsenoside R0, and araloside A is relatively slow in various tissues. In contrast, chikusetsusaponin IVa is rapidly eliminated from various tissues. The ability of four saponins to cross the blood-brain barrier is highly beneficial for the development of therapeutic drugs for central nervous system diseases. Additionally, the results from different administration routes indicate that AB saponins may exhibit a pronounced gastrointestinal and hepatic first-pass effect <em>in vivo</em>, which should be considered in future research. This study can guide multi-route study of AB saponins provides critical insights for formulation optimization and dosing regimen design to mitigate first-pass effects</div></div>","PeriodicalId":277,"journal":{"name":"Chinese Journal of Analytical Chemistry","volume":"53 7","pages":"Article 100549"},"PeriodicalIF":1.2,"publicationDate":"2025-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144154786","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}
Pub Date : 2025-04-16DOI: 10.1016/j.cjac.2025.100550
Kewei WANG , Ying ZHANG , Xilong QIAN , Zheng LIU , Weihua ZHANG , Liu ZHOU , Yanqiong PAN , Liwen ZHENG , Fang FANG , Yang ZHANG , Yehuang WANG , Bin JIANG , Shengjin LIU
Yuhuang Shengji ointment (YSO) is a traditional Chinese medicine clinical prescription from Professor Wang Yehuang, a famous Chinese medicine professor in Jiangsu Province, China. It is used for the treatment of postoperative healing of anal fistula in clinic practice. It is composed of Corydalis Rhizoma, Radix Sanguisorbae Carbonisata, Natrii Sulfas, Alumen Ustum, Plant Soot and Borneolum. It has the effects of eliminating dampness, astringing sores, hemostasis, pain relief, detumescence and muscle regeneration. According to the characteristics that YSO mainly contains inorganic, organic and volatile components, the comprehensive quality control of the ointment was achieved by different analytical methods. The organic components in the ointment were qualitatively analyzed by ultra performance liquid chromatography coupled with quadrupole time of flight mass spectrometry (UPLC-Q-TOF-MS) to determine the main chemical components. High performance liquid chromatography (HPLC) fingerprint of the organic components of the ointment was further established. Inductively coupled plasma mass spectrometry (ICP-MS) technology is used to analyze the inorganic elements in ointment, which provides data support for the quality control of inorganic components. The flash GC e-nose is used for rapid detection of volatile substances in ointment, and the fingerprint of volatile components is established. The comprehensive use of these analytical techniques not only reflects the overall chemical characteristics of the ointment, but also helps to evaluate the consistency between different batches of products. This study successfully established a comprehensive quality analysis method, which provided a basis for the quality control of YSO. At the same time, it provides a more comprehensive quality control strategy for ointment which mainly contains organic, inorganic and volatile components.
{"title":"Quality control methods established in view of the characteristics of component type of Yuhuang Shengji ointment based on HPLC, ICP-MS and GC e-nose","authors":"Kewei WANG , Ying ZHANG , Xilong QIAN , Zheng LIU , Weihua ZHANG , Liu ZHOU , Yanqiong PAN , Liwen ZHENG , Fang FANG , Yang ZHANG , Yehuang WANG , Bin JIANG , Shengjin LIU","doi":"10.1016/j.cjac.2025.100550","DOIUrl":"10.1016/j.cjac.2025.100550","url":null,"abstract":"<div><div>Yuhuang Shengji ointment (YSO) is a traditional Chinese medicine clinical prescription from Professor Wang Yehuang, a famous Chinese medicine professor in Jiangsu Province, China. It is used for the treatment of postoperative healing of anal fistula in clinic practice. It is composed of Corydalis Rhizoma, Radix Sanguisorbae Carbonisata, Natrii Sulfas, Alumen Ustum, Plant Soot and Borneolum. It has the effects of eliminating dampness, astringing sores, hemostasis, pain relief, detumescence and muscle regeneration. According to the characteristics that YSO mainly contains inorganic, organic and volatile components, the comprehensive quality control of the ointment was achieved by different analytical methods. The organic components in the ointment were qualitatively analyzed by ultra performance liquid chromatography coupled with quadrupole time of flight mass spectrometry (UPLC-Q-TOF-MS) to determine the main chemical components. High performance liquid chromatography (HPLC) fingerprint of the organic components of the ointment was further established. Inductively coupled plasma mass spectrometry (ICP-MS) technology is used to analyze the inorganic elements in ointment, which provides data support for the quality control of inorganic components. The flash GC e-nose is used for rapid detection of volatile substances in ointment, and the fingerprint of volatile components is established. The comprehensive use of these analytical techniques not only reflects the overall chemical characteristics of the ointment, but also helps to evaluate the consistency between different batches of products. This study successfully established a comprehensive quality analysis method, which provided a basis for the quality control of YSO. At the same time, it provides a more comprehensive quality control strategy for ointment which mainly contains organic, inorganic and volatile components.</div></div>","PeriodicalId":277,"journal":{"name":"Chinese Journal of Analytical Chemistry","volume":"53 7","pages":"Article 100550"},"PeriodicalIF":1.2,"publicationDate":"2025-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144169999","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}
Vanadium is considered a microelement of great industrial, environmental, biological, and pharmacological importance. Vanadium-containing complexes have been widely used as biologically active compounds. Outside cells, vanadium exists in the form of the vanadate anion, while inside cells, it primarily exists as the tetravalent vanadyl cation. Both a deficiency and an excess of vanadium in the human body can lead to various diseases. Therefore, the aim of this study is to detect vanadium (V) ions using fluorescent carbon dots, which are capable of rapid and sensitive detection. In this study, carbon dots synthesized from chitosan and melamine were used as fluorescent reagents. Fluorescent carbon dots (C-dots) were synthesized by hydrothermally treating 99.95% pure chitosan with melamine at 180 °C for 5 h, followed by freeze-drying in a lyophilizer, and purification using high performance liquid chromatography (HPLC). These dots were found to emit bright green fluorescence. The formation of green fluorescence is associated with the incorporation of nitrogen into the carbon materials, which were then used for the detection of vanadium (V) ions. The C-dots and their complexation with vanadium (V) were fully characterized by infrared spectroscopy and spectrofluorometry.
{"title":"Synthesis of carbon dots based on chitosan and melamine and their application in detecting vanadate (V) anions","authors":"Farida ALLAMBERGENOVA , Zulayho SMANOVA , Nigora QUTLIMUROTOVA , Abdurakhman ABDREYMOV , Fotima SOBIROVA , Ruhiya QUTLIMUROTOVA , Khusan YAKHSHINOROV","doi":"10.1016/j.cjac.2025.100538","DOIUrl":"10.1016/j.cjac.2025.100538","url":null,"abstract":"<div><div>Vanadium is considered a microelement of great industrial, environmental, biological, and pharmacological importance. Vanadium-containing complexes have been widely used as biologically active compounds. Outside cells, vanadium exists in the form of the vanadate anion, while inside cells, it primarily exists as the tetravalent vanadyl cation. Both a deficiency and an excess of vanadium in the human body can lead to various diseases. Therefore, the aim of this study is to detect vanadium (V) ions using fluorescent carbon dots, which are capable of rapid and sensitive detection. In this study, carbon dots synthesized from chitosan and melamine were used as fluorescent reagents. Fluorescent carbon dots (C-dots) were synthesized by hydrothermally treating 99.95% pure chitosan with melamine at 180 °C for 5 h, followed by freeze-drying in a lyophilizer, and purification using high performance liquid chromatography (HPLC). These dots were found to emit bright green fluorescence. The formation of green fluorescence is associated with the incorporation of nitrogen into the carbon materials, which were then used for the detection of vanadium (V) ions. The C-dots and their complexation with vanadium (V) were fully characterized by infrared spectroscopy and spectrofluorometry.</div></div>","PeriodicalId":277,"journal":{"name":"Chinese Journal of Analytical Chemistry","volume":"53 7","pages":"Article 100538"},"PeriodicalIF":1.2,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144090528","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}
Inspired by the advantageous properties of coumarin and thiazole fluorophores, we rationally designed and developed a novel coumarin-thiazole conjugated fluorescent probe (PC), featuring an acryloyl ester group as the triggering and responding entity for the specific identification of cysteine (Cys). Probe PC exhibited a distinct color change (colorless to bright green), a large Stokes shift, excellent sensitivity, high selectivity, and strong anti-interference capabilities. the density function theory (DFT), high-resolution mass spectrometry (HRMS), and proton nuclear magnetic resonance (1H NMR) assays further affirmed that the response mechanism encompasses an addition-cyclization reaction between the acryloyl domain of probe PC and the sulfhydryl and amino entities of Cys, engendering the liberation of a lustrous green fluorescent chromophore (PCOH) that can be visually discerned. Compared with previous reports, this is a new scaffold based on coumarin that achieves the quantitative determination of Cys in different food matrices in real-time. Furthermore, probe PC is effectively employed for visual imaging of Cys in A549 cells and five-day-old zebrafish, exhibiting low cytotoxicity and favorable cellular permeability, which demonstrated its practical application.
{"title":"A novel coumarin-thiazole conjugated ICT fluorescent probe for cysteine specific detection in food samples, living cells and zebrafish","authors":"Xiaoyan CAO, Yifan WEI, Yingyue DING, Yichi ZHANG, Chuanqing REN, Qin WANG","doi":"10.1016/j.cjac.2025.100542","DOIUrl":"10.1016/j.cjac.2025.100542","url":null,"abstract":"<div><div>Inspired by the advantageous properties of coumarin and thiazole fluorophores, we rationally designed and developed a novel coumarin-thiazole conjugated fluorescent probe (PC), featuring an acryloyl ester group as the triggering and responding entity for the specific identification of cysteine (Cys). Probe PC exhibited a distinct color change (colorless to bright green), a large Stokes shift, excellent sensitivity, high selectivity, and strong anti-interference capabilities. the density function theory (DFT), high-resolution mass spectrometry (HRMS), and proton nuclear magnetic resonance (<sup>1</sup>H NMR) assays further affirmed that the response mechanism encompasses an addition-cyclization reaction between the acryloyl domain of probe PC and the sulfhydryl and amino entities of Cys, engendering the liberation of a lustrous green fluorescent chromophore (PC<strong><img></strong>OH) that can be visually discerned. Compared with previous reports, this is a new scaffold based on coumarin that achieves the quantitative determination of Cys in different food matrices in real-time. Furthermore, probe PC is effectively employed for visual imaging of Cys in A549 cells and five-day-old zebrafish, exhibiting low cytotoxicity and favorable cellular permeability, which demonstrated its practical application.</div></div>","PeriodicalId":277,"journal":{"name":"Chinese Journal of Analytical Chemistry","volume":"53 7","pages":"Article 100542"},"PeriodicalIF":1.2,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144090661","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}
The occurrence of illicit drugs in water has been extensively reported around the world, however, limited data are available in sediments, probably due to the lack of effective and robust analytical methods. This research established a sensitive method for determining 12 illicit drugs, including amphetamine, methamphetamine, methcathinone, ephedrine, 3,4-methylenedioxy-amphetamine, 3,4-methylenedioxy-n-methamphetamine, norketamine, ketamine, benzoylecgonine, codeine, cocaine, and methadone in sediments. The combination of salt and solution (extraction step) and adsorbents (purification step) in the QuEChERS method was optimized to enhance the applicability and reliability of the analytical approach, which was subsequently combined with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The developed method demonstrated satisfactory linearity (R2 > 0.995) within 0.1 to 50 ng/g dry weight (dw), with limits of detection and quantification ranging from 0.0077 to 0.0299 ng/g dw and 0.0255 to 0.0996 ng/g dw, respectively. Recoveries of target drugs ranged from 60.5 % to 114.9 %, with intra-day and inter-day relative standard deviations below 10.9 % and 12.3 %, respectively, which are within the acceptable limits. Application of the validated method to sediments from the Beiyunhe River Basin, China revealed the presence of nine out of twelve targeted drugs. Total drug concentrations ranged from 0.12 to 1.18 ng/g dw, with ephedrine being predominant, followed by amphetamine and methadone. Ecological risk assessments indicated low biological hazards from the detected drugs to aquatic ecosystems. However, due to their high polarity and biological activity, continued attention to the ecological risks of illicit drugs would provide greater reassurance. This research presents the first application of QuEChERS for extracting illicit drugs from sediments. The optimized method elucidates these emerging contaminants' behavior and facilitates accurate environmental risk assessments. Due to its high sensitivity, good recovery and precision, the method is well-suited to routine monitoring of trace-level illicit drugs in complex sediment matrices.
{"title":"Determination of illicit drugs in sediments using a modified QuEChERS method coupled with UPLC-MS/MS","authors":"Meng ZHANG, Changsheng GUO, Heng ZHANG, Yanghui DENG, Xu TAN, Ya GAO, Jian XU","doi":"10.1016/j.cjac.2025.100540","DOIUrl":"10.1016/j.cjac.2025.100540","url":null,"abstract":"<div><div>The occurrence of illicit drugs in water has been extensively reported around the world, however, limited data are available in sediments, probably due to the lack of effective and robust analytical methods. This research established a sensitive method for determining 12 illicit drugs, including amphetamine, methamphetamine, methcathinone, ephedrine, 3,4-methylenedioxy-amphetamine, 3,4-methylenedioxy-n-methamphetamine, norketamine, ketamine, benzoylecgonine, codeine, cocaine, and methadone in sediments. The combination of salt and solution (extraction step) and adsorbents (purification step) in the QuEChERS method was optimized to enhance the applicability and reliability of the analytical approach, which was subsequently combined with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The developed method demonstrated satisfactory linearity (<em>R</em><sup>2</sup> > 0.995) within 0.1 to 50 ng/g dry weight (dw), with limits of detection and quantification ranging from 0.0077 to 0.0299 ng/g dw and 0.0255 to 0.0996 ng/g dw, respectively. Recoveries of target drugs ranged from 60.5 % to 114.9 %, with intra-day and inter-day relative standard deviations below 10.9 % and 12.3 %, respectively, which are within the acceptable limits. Application of the validated method to sediments from the Beiyunhe River Basin, China revealed the presence of nine out of twelve targeted drugs. Total drug concentrations ranged from 0.12 to 1.18 ng/g dw, with ephedrine being predominant, followed by amphetamine and methadone. Ecological risk assessments indicated low biological hazards from the detected drugs to aquatic ecosystems. However, due to their high polarity and biological activity, continued attention to the ecological risks of illicit drugs would provide greater reassurance. This research presents the first application of QuEChERS for extracting illicit drugs from sediments. The optimized method elucidates these emerging contaminants' behavior and facilitates accurate environmental risk assessments. Due to its high sensitivity, good recovery and precision, the method is well-suited to routine monitoring of trace-level illicit drugs in complex sediment matrices.</div></div>","PeriodicalId":277,"journal":{"name":"Chinese Journal of Analytical Chemistry","volume":"53 7","pages":"Article 100540"},"PeriodicalIF":1.2,"publicationDate":"2025-04-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144090663","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}
Pub Date : 2025-04-13DOI: 10.1016/j.cjac.2025.100541
Walaa GABER , Nabila SHEHATA , May BIN-JUMAH , Ahmed A. ALLAM , Wail Al ZOUBI , Mostafa R. ABUKHADRA
Magnesium-rich zeolite-A (Mg.ZA) was successfully synthesized from natural talc minerals as a novel form of magnesium silicate zeolitic structure with a surface area of 187 m2/g and mesoporous nature (1.5 to 10 nm). Different characterization techniques, including X-ray diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray spectroscopy (EDX), scanning electron microscope (SEM), and Brunner−Emmet−Teller (BET), confirmed the formation of Mg.ZA. The adsorption properties of Mg.ZA were evaluated for effective retention of toxic Cd (II) and Zn (II) metallic ions from the water supplies. The Mg.ZA structure displays significant capacities for the two ions, with saturation capacities (278 mg/g (Cd (II)) and 221.2 mg/g (Zn (II)) higher than several investigated adsorbents. Based on the steric analysis of the applied advanced isotherm models, the structure of Mg.ZA was enriched in 150 and 106.9 mg/g effective uptake sites during the retention of Cd (II) and Zn (II), respectively. Up to three ions of Cd (II) and Zn (II) can occupy each of these sites, contributing to their adsorption in a vertical orientation through multi-interaction or multi-ionic mechanisms. The energetic assessment, either based on Gaussian energy (< 7 kJ/mol) or adsorption energy (< 6 kJ/mol), suggested the predominant impact of physical mechanisms (hydrogen bonds and electrostatic attraction), in addition to the impact of the zeolitic ion exchange process (0.6 to 25 kJ/mol). Furthermore, the thermodynamic functions declare the retention of these ions into the framework of Mg.ZA by exothermic and spontaneous reactions.
{"title":"Steric and energetic studies on the retention of Cd (II) and Zn (II) metal ions into magnesium rich zeolite-A synthesized from natural talc: Experimental and theoretical studies","authors":"Walaa GABER , Nabila SHEHATA , May BIN-JUMAH , Ahmed A. ALLAM , Wail Al ZOUBI , Mostafa R. ABUKHADRA","doi":"10.1016/j.cjac.2025.100541","DOIUrl":"10.1016/j.cjac.2025.100541","url":null,"abstract":"<div><div>Magnesium-rich zeolite-A (Mg.ZA) was successfully synthesized from natural talc minerals as a novel form of magnesium silicate zeolitic structure with a surface area of 187 m<sup>2</sup>/g and mesoporous nature (1.5 to 10 nm). Different characterization techniques, including X-ray diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray spectroscopy (EDX), scanning electron microscope (SEM), and Brunner−Emmet−Teller (BET), confirmed the formation of Mg.ZA. The adsorption properties of Mg.ZA were evaluated for effective retention of toxic Cd (II) and Zn (II) metallic ions from the water supplies. The Mg.ZA structure displays significant capacities for the two ions, with saturation capacities (278 mg/g (Cd (II)) and 221.2 mg/g (Zn (II)) higher than several investigated adsorbents. Based on the steric analysis of the applied advanced isotherm models, the structure of Mg.ZA was enriched in 150 and 106.9 mg/g effective uptake sites during the retention of Cd (II) and Zn (II), respectively. Up to three ions of Cd (II) and Zn (II) can occupy each of these sites, contributing to their adsorption in a vertical orientation through multi-interaction or multi-ionic mechanisms. The energetic assessment, either based on Gaussian energy (< 7 kJ/mol) or adsorption energy (< 6 kJ/mol), suggested the predominant impact of physical mechanisms (hydrogen bonds and electrostatic attraction), in addition to the impact of the zeolitic ion exchange process (0.6 to 25 kJ/mol). Furthermore, the thermodynamic functions declare the retention of these ions into the framework of Mg.ZA by exothermic and spontaneous reactions.</div></div>","PeriodicalId":277,"journal":{"name":"Chinese Journal of Analytical Chemistry","volume":"53 6","pages":"Article 100541"},"PeriodicalIF":1.2,"publicationDate":"2025-04-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143943581","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}
Pub Date : 2025-04-10DOI: 10.1016/j.cjac.2025.100530
Ming BAI, Xuebing LI, Yawen LIU, Liwei ZHAO, Qingqi FENG, Jianlong MA
Trigonelline is an alkaloid primarily found in fenugreek (Trigonella foenum-graecum) seeds, exhibiting diverse pharmacological activities, including anti-diabetic, antioxidant, and anti-inflammatory effects. With the growing application of trigonelline in drug development and quality control, the development of efficient and accurate analytical methods is critical to ensure its proper assessment and utilization. This study aims to develop and validate a HPLC method for the precise separation and quantitative determination of trigonelline. The method utilizes a Dalian Elite Hypersil NH2 chromatographic column (250 mm × 4.6 mm, 5 µm) with a mobile phase of acetonitrile: water (70:30, v/v), a flow rate of 1.0 mL/min, column temperature maintained at 35 °C, and detection wavelength set at 264 nm. The method was applied to analyze fenugreek seed extracts prepared via ultrasonic extraction with methanol, employing a 30-minute extraction time. The results demonstrated that the method achieved an excellent linear range (R2 > 0.9999), high precision (RSD < 2 %), system suitability, and recovery rate is between 95 % and 105 %, meeting the quality standards for trigonelline analysis. In conclusion, this study introduces a reliable and efficient HPLC method, offering robust technical support for the quantitative analysis of trigonelline and the quality evaluation of related pharmaceutical products, facilitating its application in clinical drug monitoring and standardization.
葫芦巴碱是一种主要存在于葫芦巴种子中的生物碱，具有多种药理活性，包括抗糖尿病、抗氧化和抗炎作用。随着葫芦巴碱在药物开发和质量控制中的应用越来越广泛，建立高效、准确的分析方法是保证其合理评价和利用的关键。本研究旨在建立高效液相色谱法精确分离和定量测定葫芦巴碱。方法采用大连Elite Hypersil NH2色谱柱（250 mm × 4.6 mm, 5µm），流动相为乙腈：水（70:30,v/v），流速为1.0 mL/min，柱温35℃，检测波长264 nm。采用该方法对甲醇超声提取胡芦巴籽提取物进行了分析，提取时间为30分钟。结果表明，该方法具有良好的线性范围(R2 >；0.9999)，高精度(RSD <；回收率在95 % ~ 105 %之间，符合葫芦巴碱分析的质量标准。综上所述，本研究引入了一种可靠、高效的HPLC方法，为葫芦巴碱的定量分析和相关药品的质量评价提供了有力的技术支持，促进了葫芦巴碱在临床药物监测和标准化中的应用。
{"title":"Development and validation of an HPLC method for quantitative analysis of trigonelline","authors":"Ming BAI, Xuebing LI, Yawen LIU, Liwei ZHAO, Qingqi FENG, Jianlong MA","doi":"10.1016/j.cjac.2025.100530","DOIUrl":"10.1016/j.cjac.2025.100530","url":null,"abstract":"<div><div>Trigonelline is an alkaloid primarily found in fenugreek (Trigonella foenum-graecum) seeds, exhibiting diverse pharmacological activities, including anti-diabetic, antioxidant, and anti-inflammatory effects. With the growing application of trigonelline in drug development and quality control, the development of efficient and accurate analytical methods is critical to ensure its proper assessment and utilization. This study aims to develop and validate a HPLC method for the precise separation and quantitative determination of trigonelline. The method utilizes a Dalian Elite Hypersil NH<sub>2</sub> chromatographic column (250 mm × 4.6 mm, 5 µm) with a mobile phase of acetonitrile: water (70:30, <em>v</em>/<em>v</em>), a flow rate of 1.0 mL/min, column temperature maintained at 35 °C, and detection wavelength set at 264 nm. The method was applied to analyze fenugreek seed extracts prepared via ultrasonic extraction with methanol, employing a 30-minute extraction time. The results demonstrated that the method achieved an excellent linear range (<em>R</em><sup>2</sup> > 0.9999), high precision (RSD < 2 %), system suitability, and recovery rate is between 95 % and 105 %, meeting the quality standards for trigonelline analysis. In conclusion, this study introduces a reliable and efficient HPLC method, offering robust technical support for the quantitative analysis of trigonelline and the quality evaluation of related pharmaceutical products, facilitating its application in clinical drug monitoring and standardization.</div></div>","PeriodicalId":277,"journal":{"name":"Chinese Journal of Analytical Chemistry","volume":"53 6","pages":"Article 100530"},"PeriodicalIF":1.2,"publicationDate":"2025-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143922270","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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