Journal of Chromatography B最新文献

LC-HRMS profiling of Dendrobium huoshanense aqueous extract and its therapeutic effects on nonalcoholic fatty liver disease in mice through the TLR2-NF-κB and AMPK-SREBP1-SIRT1 signaling pathways

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-03-16 DOI: 10.1016/j.jchromb.2025.124563

Qiyan Lin , Ke Huang , Xiyu Ge , Menghua Ma , Wei Wang , Li Yang , Cunwu Chen , Bangxing Han , Dong Liu

Dendrobium huoshanense (DH) belongs to the Dendrobium genus of the Orchidaceae family and is a herbaceous plant that protects the liver and nourishes the Yin according to traditional Chinese Medicine (TCM) theory. This research aimed to determine the therapeutic effect and mechanisms of DH on a nonalcoholic fatty liver disease (NAFLD) mouse model and its chemical composition. For pharmacological research, the pathological damage and lipid accumulation in liver tissues were evaluated using HE and oil red staining, respectively. The differential proteins between the model and DHH groups were screened using 4D label-free quantitative proteomics, and the proteomic results were verified using Western blot. The potential mechanism was validated by metabolomic analysis. The main active ingredients in a DH aqueous extract were identified using UHPLC-Q Exactive HF HRMS. Pathological staining results showed that DH can reverse liver pathological damage and lipid accumulation in the NAFLD model. Quantitative proteomics revealed that the differential proteins were mainly associated with liver lipid deposition (LAL, AMPK, TM7SF2, SBCAD, and SIRT1), insulin resistance (GYS1, GYS2, PYGL, FoxO1, and PPAR-γ), and inflammation (TLR2 and MAPKAPK). Western blot verified the above-mentioned results. Metabolomic analysis also indicated that the DH aqueous extract ameliorated NAFLD in mice by affecting cholesterol metabolism and AMPK signaling pathway, proving its significant therapeutic effects on the NAFLD model. Sixty-five compounds were identified from DH aqueous extract by analyzing the precise molecular weight and MS/MS fragmentation pathway. The pharmacological mechanism of DH in treating NAFLD mainly involved the TLR2-NF-κB and AMPK-SREBP1-SIRT1 signaling pathways.

{"title":"LC-HRMS profiling of Dendrobium huoshanense aqueous extract and its therapeutic effects on nonalcoholic fatty liver disease in mice through the TLR2-NF-κB and AMPK-SREBP1-SIRT1 signaling pathways","authors":"Qiyan Lin , Ke Huang , Xiyu Ge , Menghua Ma , Wei Wang , Li Yang , Cunwu Chen , Bangxing Han , Dong Liu","doi":"10.1016/j.jchromb.2025.124563","DOIUrl":"10.1016/j.jchromb.2025.124563","url":null,"abstract":"<div><div><em>Dendrobium huoshanense</em> (DH) belongs to the <em>Dendrobium</em> genus of the Orchidaceae family and is a herbaceous plant that protects the liver and nourishes the Yin according to traditional Chinese Medicine (TCM) theory. This research aimed to determine the therapeutic effect and mechanisms of DH on a nonalcoholic fatty liver disease (NAFLD) mouse model and its chemical composition. For pharmacological research, the pathological damage and lipid accumulation in liver tissues were evaluated using HE and oil red staining, respectively. The differential proteins between the model and DHH groups were screened using 4D label-free quantitative proteomics, and the proteomic results were verified using Western blot. The potential mechanism was validated by metabolomic analysis. The main active ingredients in a DH aqueous extract were identified using UHPLC-Q Exactive HF HRMS. Pathological staining results showed that DH can reverse liver pathological damage and lipid accumulation in the NAFLD model. Quantitative proteomics revealed that the differential proteins were mainly associated with liver lipid deposition (LAL, AMPK, TM7SF2, SBCAD, and SIRT1), insulin resistance (GYS1, GYS2, PYGL, FoxO1, and PPAR-γ), and inflammation (TLR2 and MAPKAPK). Western blot verified the above-mentioned results. Metabolomic analysis also indicated that the DH aqueous extract ameliorated NAFLD in mice by affecting cholesterol metabolism and AMPK signaling pathway, proving its significant therapeutic effects on the NAFLD model. Sixty-five compounds were identified from DH aqueous extract by analyzing the precise molecular weight and MS/MS fragmentation pathway. The pharmacological mechanism of DH in treating NAFLD mainly involved the TLR2-NF-κB and AMPK-SREBP1-SIRT1 signaling pathways.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124563"},"PeriodicalIF":2.8,"publicationDate":"2025-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143643178","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

LAMAS 4 IC - Laboratory approved metadata acquisition schemas for ion chromatography.

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-03-13 DOI: 10.1016/j.jchromb.2025.124556

Robert Wagner, Markus M Becker, Martina Balazinski, Uta Schnabel, Harald Below, Kristina Yordanova, Dagmar Waltemath

Metadata are necessary to describe scientific experiments. The use of metadata schemas enable the collection of structured and standardized metadata, supporting the findability, accessibility, interoperability and reusability of the data and metadata in accordance with the FAIR data principles. This paper introduces the first metadata schemas for the analytical methods of anion and cation ion-exchange chromatography measurements. The developed schemas are aligned with the ASTM E1151:1993 norm defining terms and relationships in ion chromatography. They are implemented by using the common JSON schema standard and publicly shared for direct use and further refinement for various application fields of IC measurements. Approval of the schema in laboratory environments was achieved in the field of applied plasma science and two examples from different use cases of water analysis for plasma applications are represented. Through practical application, the introduced schemas have demonstrated their effectiveness in laboratory environments, marking a step forward in standardizing the documentation of IC measurements to support advanced research data management and the application of modern data science methods.

{"title":"LAMAS 4 IC - Laboratory approved metadata acquisition schemas for ion chromatography.","authors":"Robert Wagner, Markus M Becker, Martina Balazinski, Uta Schnabel, Harald Below, Kristina Yordanova, Dagmar Waltemath","doi":"10.1016/j.jchromb.2025.124556","DOIUrl":"https://doi.org/10.1016/j.jchromb.2025.124556","url":null,"abstract":"<p><p>Metadata are necessary to describe scientific experiments. The use of metadata schemas enable the collection of structured and standardized metadata, supporting the findability, accessibility, interoperability and reusability of the data and metadata in accordance with the FAIR data principles. This paper introduces the first metadata schemas for the analytical methods of anion and cation ion-exchange chromatography measurements. The developed schemas are aligned with the ASTM E1151:1993 norm defining terms and relationships in ion chromatography. They are implemented by using the common JSON schema standard and publicly shared for direct use and further refinement for various application fields of IC measurements. Approval of the schema in laboratory environments was achieved in the field of applied plasma science and two examples from different use cases of water analysis for plasma applications are represented. Through practical application, the introduced schemas have demonstrated their effectiveness in laboratory environments, marking a step forward in standardizing the documentation of IC measurements to support advanced research data management and the application of modern data science methods.</p>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"124556"},"PeriodicalIF":2.8,"publicationDate":"2025-03-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143668511","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Metabolic profiling of 5- Methoxy-N,N-diallyltryptamine in human liver microsomes and zebrafish using LC-Orbitrap MS

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-03-09 DOI: 10.1016/j.jchromb.2025.124557

Liang Meng , Yanjiao Wang , Chenhao Zhong , Sen Zhao

The metabolic profiles of tryptamine-derived new psychoactive substance 5-Methoxy-N, N-diallyltryptamine (5-MeO-DALT) were investigated using both zebrafish and human liver microsome models. The ultra-high performance liquid chromatography Q Exactive Quadrupole-Orbitrap high resolution mass spectrometer (UPLC-Q-Orbitrap-HRMS) was employed to analyze the intoxicated zebrafish samples, as well as human liver microsomes samples. The mass spectrometric data were analyzed by a software of Compound Discoverer with a database of potential metabolites. As the result, A total of 11 metabolites were generated in human liver microsome model. The main metabolic pathways of the phase I metabolism included N-Oxidation，Aromatic hydroxylation，Indole-dihydroxylation reaction，N-Dealkylation and aromatic hydroxylation，N-Dealkylation and O-demethylation，Aromatic hydroxylation and O-demethylation and Hydration and N-oxidation. Meanwhile the phase II metabolism included Glucuronidation following O-demethylation，Glucuronidation following aromatic hydroxylation. A total of 8 metabolites were generated in zebrafish model. The main metabolic pathways of the phase I metabolism included Aromatic hydroxylation, N-Dehydrogenation, N-Dealkylation, N-Dealkylation and aromatic hydroxylation, meanwhile the phase II metabolism included Sulfonation following aromatic hydroxylation, Glucuronidation following aromatic hydroxylation, Sulfonation following O-demethylation. The phase I metabolites 5-MeO-DALT-Aromatic hydroxylation, 5-MeO-DALT-N-Depropylation and the phase II metabolite OH&Glucuronidation conjugation-5-MeO-DALT, OH& Sulfonation conjugation-5-MeO-DALT were proposed to be appropriate markers for 5-MeO-DAPT intake for screening, while the inclusion of the parent drug itself and OH&Glucuronidation conjugation-5-MeO-DALT may be useful for confirmation purposes.

{"title":"Metabolic profiling of 5- Methoxy-N,N-diallyltryptamine in human liver microsomes and zebrafish using LC-Orbitrap MS","authors":"Liang Meng , Yanjiao Wang , Chenhao Zhong , Sen Zhao","doi":"10.1016/j.jchromb.2025.124557","DOIUrl":"10.1016/j.jchromb.2025.124557","url":null,"abstract":"<div><div>The metabolic profiles of tryptamine-derived new psychoactive substance 5-Methoxy-N, N-diallyltryptamine (5-MeO-DALT) were investigated using both zebrafish and human liver microsome models. The ultra-high performance liquid chromatography Q Exactive Quadrupole-Orbitrap high resolution mass spectrometer (UPLC-Q-Orbitrap-HRMS) was employed to analyze the intoxicated zebrafish samples, as well as human liver microsomes samples. The mass spectrometric data were analyzed by a software of Compound Discoverer with a database of potential metabolites. As the result, A total of 11 metabolites were generated in human liver microsome model. The main metabolic pathways of the phase I metabolism included N-Oxidation，Aromatic hydroxylation，Indole-dihydroxylation reaction，N-Dealkylation and aromatic hydroxylation，N-Dealkylation and <em>O</em>-demethylation，Aromatic hydroxylation and <em>O</em>-demethylation and Hydration and N-oxidation. Meanwhile the phase II metabolism included Glucuronidation following <em>O</em>-demethylation，Glucuronidation following aromatic hydroxylation. A total of 8 metabolites were generated in zebrafish model. The main metabolic pathways of the phase I metabolism included Aromatic hydroxylation, N-Dehydrogenation, N-Dealkylation, N-Dealkylation and aromatic hydroxylation, meanwhile the phase II metabolism included Sulfonation following aromatic hydroxylation, Glucuronidation following aromatic hydroxylation, Sulfonation following <em>O</em>-demethylation. The phase I metabolites 5-MeO-DALT-Aromatic hydroxylation, 5-MeO-DALT-N-Depropylation and the phase II metabolite OH&Glucuronidation conjugation-5-MeO-DALT, OH& Sulfonation conjugation-5-MeO-DALT were proposed to be appropriate markers for 5-MeO-DAPT intake for screening, while the inclusion of the parent drug itself and OH&Glucuronidation conjugation-5-MeO-DALT may be useful for confirmation purposes.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124557"},"PeriodicalIF":2.8,"publicationDate":"2025-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143601358","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Total ginsenosides from wild ginseng improve immune regulation in a rat model of spleen qi deficiency by modulating fecal-bacteria-associated short-chain fatty acids and intestinal barrier integrity

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-03-06 DOI: 10.1016/j.jchromb.2025.124554

Ruobing Bai , Liting Ma , Fangtong Li , Lijia Pan , Yuwen Bao , Xinze Li , Shen Wang , Hao Yue , Fei Zheng

For thousands of years, traditional Chinese medicine (TCM) has made extensive use of wild ginseng. It is thought to provide vital energy effects and to boost immunity. This study aimed to clarify the processes by which short-chain fatty acids (SCFAs) metabolites and the intestinal barrier are used by total ginsenosides wild ginseng (TWG) to modulate immunity. In this study, we analyzed and identified ginsenosides in the colon using UPLC-Q-TOF-MS^E methods. In the meantime, a rat model of spleen qi deficiency (SQD) was created using reserpine, and the effects of TWG on intestinal barrier function and short-chain fatty acids in the feces of SQD-affected rats were examined. 28 ginsenosides were found in the colon during this experiment, and the main components were measured. TWG considerably increased fecal concentrations of acetic, propionic and 6 others, according to SCFAs analysis. According to serum immunological markers, TWG reduced IL-17 and IL-1β levels, increased IL-10, IL-22, and TGF-β concentrations, balanced Th17/Treg ratios, and reduced toxicants such DAO and LPS in rats with SQD. TWG improved barrier function, reduced permeability, increased tight junction protein expression, and lessened intestinal injury. A favorable correlation between intestinal barrier proteins and fatty acids was shown by correlation studies. The gut barrier and SCFAs perspectives helped to clarify the mechanism by which TWG controls immune activity. This study offers a fresh theoretical framework for TWG's future advancement and application.

{"title":"Total ginsenosides from wild ginseng improve immune regulation in a rat model of spleen qi deficiency by modulating fecal-bacteria-associated short-chain fatty acids and intestinal barrier integrity","authors":"Ruobing Bai , Liting Ma , Fangtong Li , Lijia Pan , Yuwen Bao , Xinze Li , Shen Wang , Hao Yue , Fei Zheng","doi":"10.1016/j.jchromb.2025.124554","DOIUrl":"10.1016/j.jchromb.2025.124554","url":null,"abstract":"<div><div>For thousands of years, traditional Chinese medicine (TCM) has made extensive use of wild ginseng. It is thought to provide vital energy effects and to boost immunity. This study aimed to clarify the processes by which short-chain fatty acids (SCFAs) metabolites and the intestinal barrier are used by total ginsenosides wild ginseng (TWG) to modulate immunity. In this study, we analyzed and identified ginsenosides in the colon using UPLC-Q-TOF-MS<sup>E</sup> methods. In the meantime, a rat model of spleen qi deficiency (SQD) was created using reserpine, and the effects of TWG on intestinal barrier function and short-chain fatty acids in the feces of SQD-affected rats were examined. 28 ginsenosides were found in the colon during this experiment, and the main components were measured. TWG considerably increased fecal concentrations of acetic, propionic and 6 others, according to SCFAs analysis. According to serum immunological markers, TWG reduced IL-17 and IL-1β levels, increased IL-10, IL-22, and TGF-β concentrations, balanced Th17/Treg ratios, and reduced toxicants such DAO and LPS in rats with SQD. TWG improved barrier function, reduced permeability, increased tight junction protein expression, and lessened intestinal injury. A favorable correlation between intestinal barrier proteins and fatty acids was shown by correlation studies. The gut barrier and SCFAs perspectives helped to clarify the mechanism by which TWG controls immune activity. This study offers a fresh theoretical framework for TWG's future advancement and application.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124554"},"PeriodicalIF":2.8,"publicationDate":"2025-03-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143601545","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Establishment and application of a rapid method for the determination of both total and unbound anlotinib concentrations by high-performance liquid chromatography–tandem mass spectrometry

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-03-05 DOI: 10.1016/j.jchromb.2025.124555

Min Zhang , Haichi Song , Zhongzhen Yuan , Tiantian Tang , Qiaoqiao Li , Jin Zeng , Lixian Li , Wanyi Chen

The unbound concentration of anlotinib is closely associated with its therapeutic efficacy and adverse reactions. In this study, we established an accurate and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the detection of total and unbound concentrations of anlotinib, which was subsequently applied to clinical samples. The separation of unbound and protein-bound anlotinib was achieved through filtration-ultrafiltration (CF-UF). Anlotinib-d5 served as the internal standard, and protein precipitation was utilized for sample preparation. The final method was thoroughly validated over a concentration range of 0.5–200 ng/mL according to related regulatory guidelines. Additionally, we demonstrated the clinical value of this method by analyzing blood samples from 39 lung cancer patients to quantify both total and unbound anlotinib concentrations. This method provides a foundation for further research into the relationship between anlotinib concentrations, therapeutic efficacy, and adverse reactions, ultimately facilitating the optimization of treatment strategies for patients.

{"title":"Establishment and application of a rapid method for the determination of both total and unbound anlotinib concentrations by high-performance liquid chromatography–tandem mass spectrometry","authors":"Min Zhang , Haichi Song , Zhongzhen Yuan , Tiantian Tang , Qiaoqiao Li , Jin Zeng , Lixian Li , Wanyi Chen","doi":"10.1016/j.jchromb.2025.124555","DOIUrl":"10.1016/j.jchromb.2025.124555","url":null,"abstract":"<div><div>The unbound concentration of anlotinib is closely associated with its therapeutic efficacy and adverse reactions. In this study, we established an accurate and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the detection of total and unbound concentrations of anlotinib, which was subsequently applied to clinical samples. The separation of unbound and protein-bound anlotinib was achieved through filtration-ultrafiltration (CF-UF). Anlotinib-d5 served as the internal standard, and protein precipitation was utilized for sample preparation. The final method was thoroughly validated over a concentration range of 0.5–200 ng/mL according to related regulatory guidelines. Additionally, we demonstrated the clinical value of this method by analyzing blood samples from 39 lung cancer patients to quantify both total and unbound anlotinib concentrations. This method provides a foundation for further research into the relationship between anlotinib concentrations, therapeutic efficacy, and adverse reactions, ultimately facilitating the optimization of treatment strategies for patients.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124555"},"PeriodicalIF":2.8,"publicationDate":"2025-03-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143592419","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Determination of seven precursor substances of 1-phenyl-2-propanone in atmospheric particulate matter by LC-MS/MS: A novel strategy for monitoring illicit drug synthesis and assessing potential health risks

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-03-05 DOI: 10.1016/j.jchromb.2025.124553

Panpan Chen , Wu Wen , Xueyan Liu , Tingting Zhang , Hongxian Yang , Mengxiang Su , Jie Chen

In the process of illicit drug production and manufacture, some of the precursors might escape into the air and adhere to the surface of airborne particulate matter. The detection of precursor substances in atmospheric particulate matter in the vicinity of suspected drug manufacturing facilities can assist in the deduction of drug synthesis pathways and the reduction of illicit drug preparation at the source. In recent years, there has been a notable transition in methamphetamine synthesis from the ephedrine/pseudoephedrine-based route to the 1-phenyl-2-propanone (P2P)-based route, underscoring the growing significance of P2P and its precursor chemicals in the surveillance and control of illicit drug manufacturing. In this study, airborne particulate matter was enriched using an atmospheric particulate matter sampler, and the samples were processed by wet milling method. A quantitative method for the detection of seven precursor substances of P2P was established by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The results showed that the limits of detection for the seven precursor substances of P2P were in the range of 0.20–0.50 ng/mL, and the linear correlation coefficients (r) were all greater than 0.9940. The matrix effects and recovery at three spiked levels were in the ranges of 92.1 %–107.4 % and 94.0 %–105.2 %, respectively. Utilising this method to collect the actual samples from the laboratory, 3-oxo-2-phenylbutanamide (APAA) was detected in the in vitro sample weighing room and was identified at a concentration of 91.5 pg/m³ on the initial day of collection. It was determined that the maximum possible daily inhalation dose of APAA for room occupants was 1.83 × 10⁻⁶ mg. Subsequently, a nonlinear function correlating concentration and collection date was fitted, laying the research foundation for combating the illicit preparation of methamphetamine synthesised via P2P and highlighting the occupational exposure of anti-drug personnel and health threat to nearby residents due to high-concentration, drug-related atmospheric particulate matter.

{"title":"Determination of seven precursor substances of 1-phenyl-2-propanone in atmospheric particulate matter by LC-MS/MS: A novel strategy for monitoring illicit drug synthesis and assessing potential health risks","authors":"Panpan Chen , Wu Wen , Xueyan Liu , Tingting Zhang , Hongxian Yang , Mengxiang Su , Jie Chen","doi":"10.1016/j.jchromb.2025.124553","DOIUrl":"10.1016/j.jchromb.2025.124553","url":null,"abstract":"<div><div>In the process of illicit drug production and manufacture, some of the precursors might escape into the air and adhere to the surface of airborne particulate matter. The detection of precursor substances in atmospheric particulate matter in the vicinity of suspected drug manufacturing facilities can assist in the deduction of drug synthesis pathways and the reduction of illicit drug preparation at the source. In recent years, there has been a notable transition in methamphetamine synthesis from the ephedrine/pseudoephedrine-based route to the 1-phenyl-2-propanone (P2P)-based route, underscoring the growing significance of P2P and its precursor chemicals in the surveillance and control of illicit drug manufacturing. In this study, airborne particulate matter was enriched using an atmospheric particulate matter sampler, and the samples were processed by wet milling method. A quantitative method for the detection of seven precursor substances of P2P was established by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The results showed that the limits of detection for the seven precursor substances of P2P were in the range of 0.20–0.50 ng/mL, and the linear correlation coefficients (<em>r</em>) were all greater than 0.9940. The matrix effects and recovery at three spiked levels were in the ranges of 92.1 %–107.4 % and 94.0 %–105.2 %, respectively. Utilising this method to collect the actual samples from the laboratory, 3-oxo-2-phenylbutanamide (APAA) was detected in the in vitro sample weighing room and was identified at a concentration of 91.5 pg/m<sup>3</sup> on the initial day of collection. It was determined that the maximum possible daily inhalation dose of APAA for room occupants was 1.83 × 10<sup>−6</sup> mg. Subsequently, a nonlinear function correlating concentration and collection date was fitted, laying the research foundation for combating the illicit preparation of methamphetamine synthesised via P2P and highlighting the occupational exposure of anti-drug personnel and health threat to nearby residents due to high-concentration, drug-related atmospheric particulate matter.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124553"},"PeriodicalIF":2.8,"publicationDate":"2025-03-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143579725","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Simultaneous quantification of four urinary biomarkers related to oxidative stress using UHPLC-QqQ-MS/MS

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-03-03 DOI: 10.1016/j.jchromb.2025.124552

Yingfeng Gao, Ruiwei Xu, Huixia Liu, Shuyu Jia, Yi Zhang, Xin Meng, Jicheng Gong

Oxidative stress biomarkers have been associated with both acute and chronic health outcomes. However, traditional methods analyze different biomarkers separately, resulting in complex sample preparation, high sample consumption, lengthy processing time, and limited comparability. In this study, we presented a newly developed and validated method for the simultaneous determination of oxidative stress from multiple perspectives (DNA, lipids, and antioxidants). Using a one-step solid-phase extraction and ultra-high-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (UHPLC-QqQ-MS/MS), we measured four oxidative stress related biomarkers in urine simultaneously, within a run time of only 12 min. These biomarkers included 8-hydroxy-2′-deoxyguanosine (8-OHdG), 6-sulfatoxymelatonin (aMT6s), 8-isoprostaglandin-F_2α (8-isoPGF_2α), and 11-dehydro thromboxane B₂ (11-DH-TXB₂). The calibration curves showed wide linear ranges (0.4–800 ng/mL for 8-OHdG, 0.2–600 ng/mL for aMT6s, 0.4–600 ng/mL for 8-isoPGF_2α, and 0.4–600 ng/mL for 11-DH-TXB₂), with r² values above 0.9932 for all analytes. The method demonstrated excellent sensitivity, with detection limits below 0.12 ng/mL, and good precision, with intra- and inter-day coefficients of variation ranging from 1.2 % to 14.4 %. We applied this method to urine samples from two populations living at different altitudes and found significantly higher levels of both 8-OHdG and 11-DH-TXB₂ in the high-altitude group, likely due to hypobaric hypoxia. In the future, this new method could be applied in large-scale epidemiological studies to investigate biological mechanisms of oxidative stress in health risks or for clinical diagnosis.

{"title":"Simultaneous quantification of four urinary biomarkers related to oxidative stress using UHPLC-QqQ-MS/MS","authors":"Yingfeng Gao, Ruiwei Xu, Huixia Liu, Shuyu Jia, Yi Zhang, Xin Meng, Jicheng Gong","doi":"10.1016/j.jchromb.2025.124552","DOIUrl":"10.1016/j.jchromb.2025.124552","url":null,"abstract":"<div><div>Oxidative stress biomarkers have been associated with both acute and chronic health outcomes. However, traditional methods analyze different biomarkers separately, resulting in complex sample preparation, high sample consumption, lengthy processing time, and limited comparability. In this study, we presented a newly developed and validated method for the simultaneous determination of oxidative stress from multiple perspectives (DNA, lipids, and antioxidants). Using a one-step solid-phase extraction and ultra-high-performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (UHPLC-QqQ-MS/MS), we measured four oxidative stress related biomarkers in urine simultaneously, within a run time of only 12 min. These biomarkers included 8-hydroxy-2′-deoxyguanosine (8-OHdG), 6-sulfatoxymelatonin (aMT6s), 8-isoprostaglandin-F<sub>2α</sub> (8-isoPGF<sub>2α</sub>), and 11-dehydro thromboxane B<sub>2</sub> (11-DH-TXB<sub>2</sub>). The calibration curves showed wide linear ranges (0.4–800 ng/mL for 8-OHdG, 0.2–600 ng/mL for aMT6s, 0.4–600 ng/mL for 8-isoPGF<sub>2α</sub>, and 0.4–600 ng/mL for 11-DH-TXB<sub>2</sub>), with r<sup>2</sup> values above 0.9932 for all analytes. The method demonstrated excellent sensitivity, with detection limits below 0.12 ng/mL, and good precision, with intra- and inter-day coefficients of variation ranging from 1.2 % to 14.4 %. We applied this method to urine samples from two populations living at different altitudes and found significantly higher levels of both 8-OHdG and 11-DH-TXB<sub>2</sub> in the high-altitude group, likely due to hypobaric hypoxia. In the future, this new method could be applied in large-scale epidemiological studies to investigate biological mechanisms of oxidative stress in health risks or for clinical diagnosis.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1256 ","pages":"Article 124552"},"PeriodicalIF":2.8,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143562027","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Identification, synthesis, isolation, and characterization of formulation related degradation impurity of Cefadroxil Oral suspension

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-02-28 DOI: 10.1016/j.jchromb.2025.124537

Sunil Ramrao Murkute , Surenehalli Gowdra Vasantharaju , Girij P. Singh , Krishnamurthy Bhat , Himanshu M. Godbole , Pritesh R. Upadhyay , Anurag Trivedi

Cefadroxil is an orally active, first-generation cephalosporin antibiotic utilized in the treatment of bronchitis, pharyngitis, tonsillitis, urinary tract infections, uncomplicated skin infections, bones, and joints (de Marco and Salgado, 2017 [1]). Cefadroxil for oral suspension is formulated as dry powder for oral suspension. After reconstitution during 14 days storage, we observed an unknown impurity at relative retention time (RRT) 1.29 in cefadroxil oral suspension. The observed level of an unknown impurity was greater than 0.1 % in high-performance liquid chromatography (HPLC) analysis. The present work is focused on the identification, synthesis, and characterization of the unknown impurity by employing several sophisticated analytical techniques. Such as High-resolution mass spectroscopy (HRMS), One dimensional (1D) and two dimensional (2D) nuclear magnetic resonance spectroscopy.

引用次数: 0

Profiling neuroactive steroids in pregnancy. A non-derivatised liquid chromatography tandem mass spectrometry method for the quantitation of allopregnanolone and four related isomers in maternal serum.

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-02-27 DOI: 10.1016/j.jchromb.2025.124541

Edward Hinchliffe , Alexander Heazell

Neuroactive steroids are metabolites of progesterone, synthesised during pregnancy by the placenta. Here, we describe development of a novel liquid chromatography tandem mass spectrometry (LC-MS/MS) assay for quantitation of allopregnanolone, pregnanolone, isopregnanolone, epipregnanolone and allopregnan-20α-ol-3-one in maternal serum. Following addition of deuterated internal standards, 200 μL of serum was subjected to solid phase extraction. Chromatography was performed using a pentafluorophenyl column, and LC-MS/MS on a Sciex 6500+. Sample injection volume was 20 μL, and injection-to-injection time 10.0 min. The assay was validated according to published guidelines; assay linearity and lower limit of quantification were suitable for analysis of each steroid in maternal serum, for all analytes mean recoveries were 100 % ± 15 %, intra- and inter-assay imprecision <15 %, and matrix effects negligible, and specificity experiments confirmed nil interference from a wide range of endogenous metabolites of progesterone. The method was applied to human serum samples obtained from a large cohort of third trimester pregnancies which were subsequently characterised by normal fetal and maternal outcomes, and relationships between maternal neuroactive steroid concentrations and fetal gestational age assessed. Positive correlations between maternal serum concentration and fetal gestational age were observed for isopregnanolone, allopregnanolone and allopregnan-20α-ol-3-one. The LC-MS/MS method offers significant advantages over previously published approaches for quantitation of neuroactive steroids in human maternal serum, notably obviating the need for derivatisation, whilst achieving exceptional specificity. Characterisation of normal maternal neuroactive steroid concentrations will aid future research as dysregulated placental progesterone metabolism is observed in pregnancies with poor outcomes.

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引用次数: 0

Optimizing nuclease treatment to enhance anion exchange chromatography of HIV-derived virus-like particles

IF 2.8 3区医学 Q2 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography B

Pub Date : 2025-02-27 DOI: 10.1016/j.jchromb.2025.124539

M.S. von Elling-Tammen , F. Taft , V. Thom , J. Stitz , S. Barbe , A. Krause

Residual host cell chromatin imposes numerous challenges on purifying HIV-derived enveloped virus-like particles (VLPs) using anion-exchange chromatography (AEX). According to FDA guidelines, DNA must be reduced to less than 10 ng per dose at a fragment size of less than 200 bp. To prove the fulfillment of these quality criteria, methods for the qualitative and quantitative analysis of DNA fragments must be applied and adapted to chromatin. DNA and chromatin impede the purification of HIV VLPs with AEX, co-eluting in the same fractions as the VLPs. Although nuclease treatments can be employed, the chromatin structure can shield DNA from nuclease activity. To address these challenges, we adjusted our analytical focus on characterizing the chromatin in our clarified HIV VLP supernatant. We identified two DNA subpopulations: a main large fragment population and a minor population consisting of short fragments below 200 bp. Our findings demonstrated that the larger DNA fragments are the primary issue in our process, as they co-elute with the desired VLPs. To remove the long DNA fragment population, we optimized the nuclease treatment using a Design of Experiment approach to digest the DNA despite the tight chromatin structure. The nucleases Benzonase, Denarase, and M-SAN efficiently digested the DNA removing over 90 % of the DNA. By shredding the long DNA fragments before the AEX step, we successfully separated the HIV VLPs from the remaining short DNA fragments. Combined with nuclease treatment, AEX membrane chromatography offers an efficient single-step purification platform for HIV VLP-based vaccines and other therapeutics.

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引用次数: 0