Journal of pharmaceutical and biomedical analysis最新文献

英文中文

MALDI MSI-based spatial amine metabolomics revealing the protective effect of combination therapy against cerebral ischemia/reperfusion-induced brain injury in rats

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-01-31 DOI: 10.1016/j.jpba.2025.116715

Kening Li , Siyu Wang , Weiwei Tang , Yanwen Chen , Bin Li

Complex amine metabolic disorders are implicated in ischemic stroke and can further exacerbate brain damage. Therefore, ameliorating their metabolic disorder would be an effective way to improve recovery from brain damage after ischemia/reperfusion (I/R) injury. In this work, the protective effects of Edaravone (Eda), Ginaton injection (Gin), and their combination (Eda+Gin) against cerebral I/R injury in a middle cerebral artery occlusion/reperfusion (MCAO/R) rat model were preliminarily investigated from the perspective of spatial metabolomics. Compared to single-drug treatment, the optimized combination treatment with Eda and Gin significantly decreased infarct volumes, improved neurological function, and inhibited neuronal damage and glial cell activation in MCAO/R rats. Also, combination treatment could prolong the blood circulation time of quercetin, ginkgolide C, and eight flavonoid glycosides compared to Gin treatment alone. More importantly, the spatial metabolic alterations of amine metabolites in MCAO/R rats before and after drug treatment were comprehensively interrogated using matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI MSI) coupled with laser-assisted chemical transfer (LACT)-based on tissue chemical derivatization, such as amino acids, dipeptides, tripeptides, neurotransmitters, and the other amine metabolites. MALDI MSI results showed that the drastic metabolic disorders occurred in the cerebral cortex (CTX) and striatum (STR) and combination treatment exerted a better regulatory effect on the perturbed spatial amine metabolism. Therefore, combination treatment with Eda and Gin could significantly reduce ischemic brain damage and correct spatial metabolic disorders of amine metabolites, providing a potential treatment strategy for cerebral I/R injury.

{"title":"MALDI MSI-based spatial amine metabolomics revealing the protective effect of combination therapy against cerebral ischemia/reperfusion-induced brain injury in rats","authors":"Kening Li , Siyu Wang , Weiwei Tang , Yanwen Chen , Bin Li","doi":"10.1016/j.jpba.2025.116715","DOIUrl":"10.1016/j.jpba.2025.116715","url":null,"abstract":"<div><div>Complex amine metabolic disorders are implicated in ischemic stroke and can further exacerbate brain damage. Therefore, ameliorating their metabolic disorder would be an effective way to improve recovery from brain damage after ischemia/reperfusion (I/R) injury. In this work, the protective effects of Edaravone (Eda), Ginaton injection (Gin), and their combination (Eda+Gin) against cerebral I/R injury in a middle cerebral artery occlusion/reperfusion (MCAO/R) rat model were preliminarily investigated from the perspective of spatial metabolomics. Compared to single-drug treatment, the optimized combination treatment with Eda and Gin significantly decreased infarct volumes, improved neurological function, and inhibited neuronal damage and glial cell activation in MCAO/R rats. Also, combination treatment could prolong the blood circulation time of quercetin, ginkgolide C, and eight flavonoid glycosides compared to Gin treatment alone. More importantly, the spatial metabolic alterations of amine metabolites in MCAO/R rats before and after drug treatment were comprehensively interrogated using matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI MSI) coupled with laser-assisted chemical transfer (LACT)-based on tissue chemical derivatization, such as amino acids, dipeptides, tripeptides, neurotransmitters, and the other amine metabolites. MALDI MSI results showed that the drastic metabolic disorders occurred in the cerebral cortex (CTX) and striatum (STR) and combination treatment exerted a better regulatory effect on the perturbed spatial amine metabolism. Therefore, combination treatment with Eda and Gin could significantly reduce ischemic brain damage and correct spatial metabolic disorders of amine metabolites, providing a potential treatment strategy for cerebral I/R injury.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"257 ","pages":"Article 116715"},"PeriodicalIF":3.1,"publicationDate":"2025-01-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143162178","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 eighteen therapeutic oral anticoagulants, rodenticides, and antiplatelet agents by LC-MS/MS and its application in post-mortem forensic cases

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-01-31 DOI: 10.1016/j.jpba.2025.116709

Angélique Drague , Jean Escal , Carolyne Bidat , Sandrine Dellinger , Sophie Hodin , Sébastien Duband , Catherine Feliu , Xavier Delavenne

Anticoagulants and antiplatelet agents, which interfere with blood coagulation, can lead to fatal bleeding. Moreover, their widespread use as drugs or rodenticides poses a high risk of accidental or intentional poisoning. Therefore, quantifying these substances is essential in forensic investigations. This research aimed to develop and validate a liquid chromatography-tandem mass spectrometry method capable of quantifying eighteen anticoagulant or antiplatelet compounds (apixaban, rivaroxaban, dabigatran, warfarin, acenocoumarol, fluindione, brodifacoum, bromadiolone, difenacoum, difethialone, chlorophacinone, coumatetralyl, flocoumafen, acetylsalicylic acid, clopidogrel, dipyridamole, ticagrelor, and ticlopidine) in a single run with simple sample preparation. The method was validated according to the FDA recommendations for all compounds, with an eight-min run time in human whole blood, the gold standard in toxicological forensic investigation. The method was also validated for therapeutic compounds and most rodenticides in bile and vitreous humor. Following validation, the method was applied to seven forensic cases with a known history of anticoagulant or antiplatelet agent use to prove the validity of the method. This method provides a valuable tool for legal contexts where precise determination of anticoagulant compound presence and concentration is required.

{"title":"Simultaneous quantification of eighteen therapeutic oral anticoagulants, rodenticides, and antiplatelet agents by LC-MS/MS and its application in post-mortem forensic cases","authors":"Angélique Drague , Jean Escal , Carolyne Bidat , Sandrine Dellinger , Sophie Hodin , Sébastien Duband , Catherine Feliu , Xavier Delavenne","doi":"10.1016/j.jpba.2025.116709","DOIUrl":"10.1016/j.jpba.2025.116709","url":null,"abstract":"<div><div>Anticoagulants and antiplatelet agents, which interfere with blood coagulation, can lead to fatal bleeding. Moreover, their widespread use as drugs or rodenticides poses a high risk of accidental or intentional poisoning. Therefore, quantifying these substances is essential in forensic investigations. This research aimed to develop and validate a liquid chromatography-tandem mass spectrometry method capable of quantifying eighteen anticoagulant or antiplatelet compounds (apixaban, rivaroxaban, dabigatran, warfarin, acenocoumarol, fluindione, brodifacoum, bromadiolone, difenacoum, difethialone, chlorophacinone, coumatetralyl, flocoumafen, acetylsalicylic acid, clopidogrel, dipyridamole, ticagrelor, and ticlopidine) in a single run with simple sample preparation. The method was validated according to the FDA recommendations for all compounds, with an eight-min run time in human whole blood, the gold standard in toxicological forensic investigation. The method was also validated for therapeutic compounds and most rodenticides in bile and vitreous humor. Following validation, the method was applied to seven forensic cases with a known history of anticoagulant or antiplatelet agent use to prove the validity of the method. This method provides a valuable tool for legal contexts where precise determination of anticoagulant compound presence and concentration is required.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"257 ","pages":"Article 116709"},"PeriodicalIF":3.1,"publicationDate":"2025-01-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143080270","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

A preliminary study on estimation of postmortem submersion interval of rat cadavers in freshwater through polyamine analysis in tissues

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-01-31 DOI: 10.1016/j.jpba.2025.116706

Pei Zhang , Wei Xia , Yang Bai , Fuyuan Zhang , Yan Zhang , Wei Jiang , Huiya Yuan

The estimation of postmortem submersion interval (PMSI) has always been an important scientific issue to be addressed in drowning cases. Traditional methods, such as corpse temperature analysis and the assessment of corpse surface corruption, have limitations and cannot meet the need for accurate estimation of the time of death in the mid to late stages. Biogenic amines, as small molecules produced by protein degradation after death, have a certain regularity in relation to PMSI. To further explore the possibility of utilizing polyamines to estimate PMSI, this experiment constructed a rat cadaver model in both laboratory constant-temperature water and natural water bodies. Furthermore, cadaverine and putrescine in the liver and skeletal muscle were detected at different PMSI using gas chromatography-mass spectrometry (GC-MS). Through statistical analysis, we have constructed eight sets of mathematical models for polyamines-PMSI estimation, and determined the applicable time range through derivative analysis. After evaluation the models, the error rate in inferring PMSI using the fitted equations was less than 30 % within 242 h. The models established in this study could accurately infer PMSI in the mid to late stages of the postmortem period, providing a feasible approach for the drowning forensic issue.

{"title":"A preliminary study on estimation of postmortem submersion interval of rat cadavers in freshwater through polyamine analysis in tissues","authors":"Pei Zhang , Wei Xia , Yang Bai , Fuyuan Zhang , Yan Zhang , Wei Jiang , Huiya Yuan","doi":"10.1016/j.jpba.2025.116706","DOIUrl":"10.1016/j.jpba.2025.116706","url":null,"abstract":"<div><div>The estimation of postmortem submersion interval (PMSI) has always been an important scientific issue to be addressed in drowning cases. Traditional methods, such as corpse temperature analysis and the assessment of corpse surface corruption, have limitations and cannot meet the need for accurate estimation of the time of death in the mid to late stages. Biogenic amines, as small molecules produced by protein degradation after death, have a certain regularity in relation to PMSI. To further explore the possibility of utilizing polyamines to estimate PMSI, this experiment constructed a rat cadaver model in both laboratory constant-temperature water and natural water bodies. Furthermore, cadaverine and putrescine in the liver and skeletal muscle were detected at different PMSI using gas chromatography-mass spectrometry (GC-MS). Through statistical analysis, we have constructed eight sets of mathematical models for polyamines-PMSI estimation, and determined the applicable time range through derivative analysis. After evaluation the models, the error rate in inferring PMSI using the fitted equations was less than 30 % within 242 h. The models established in this study could accurately infer PMSI in the mid to late stages of the postmortem period, providing a feasible approach for the drowning forensic issue.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"257 ","pages":"Article 116706"},"PeriodicalIF":3.1,"publicationDate":"2025-01-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143161412","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

LC-MS/MS method for the simultaneous quantification of thiafentanil and naltrexone in bovine muscle, liver and kidney

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-01-30 DOI: 10.1016/j.jpba.2025.116711

Judith T. Christie , Mieghan Bruce , Silke Pfitzer , Liesel Laubscher , Jacobus P. Raath , Michael Laurence , Tracy Kellermann

Thiafentanil is a µ-opioid agonist used for the chemical immobilisation of a variety of ungulate species and is antagonised by the administration of naltrexone. The potential for these ungulates to be hunted for consumption by humans or predators raises concerns of drug residues in animal tissues. No analytical method to quantify tissue residue concentrations of thiafentanil has been previously reported. This research developed an LC-MS/MS method to quantify thiafentanil in bovine muscle, and both thiafentanil and naltrexone in bovine liver and kidney matrices. The analytical method was applied to quantify tissue residues in samples collected from goats 1, 2, 3, and 6 days post thiafentanil administration. The assay was validated over the calibration range 6.25–200 ng/mg for thiafentanil in muscle, and 3.13–400 ng/mg for thiafentanil and 57.8–7400 ng/mg for naltrexone in liver and kidney. No residues above the lowest limit of quantification were detected in the injection site, longissimus dorsi muscle, liver or kidney samples collected from the goats. The reported analytical method and residue depletion data provide a foundation for future thiafentanil and naltrexone residue depletion studies in wildlife species.

{"title":"LC-MS/MS method for the simultaneous quantification of thiafentanil and naltrexone in bovine muscle, liver and kidney","authors":"Judith T. Christie , Mieghan Bruce , Silke Pfitzer , Liesel Laubscher , Jacobus P. Raath , Michael Laurence , Tracy Kellermann","doi":"10.1016/j.jpba.2025.116711","DOIUrl":"10.1016/j.jpba.2025.116711","url":null,"abstract":"<div><div>Thiafentanil is a µ-opioid agonist used for the chemical immobilisation of a variety of ungulate species and is antagonised by the administration of naltrexone. The potential for these ungulates to be hunted for consumption by humans or predators raises concerns of drug residues in animal tissues. No analytical method to quantify tissue residue concentrations of thiafentanil has been previously reported. This research developed an LC-MS/MS method to quantify thiafentanil in bovine muscle, and both thiafentanil and naltrexone in bovine liver and kidney matrices. The analytical method was applied to quantify tissue residues in samples collected from goats 1, 2, 3, and 6 days post thiafentanil administration. The assay was validated over the calibration range 6.25–200 ng/mg for thiafentanil in muscle, and 3.13–400 ng/mg for thiafentanil and 57.8–7400 ng/mg for naltrexone in liver and kidney. No residues above the lowest limit of quantification were detected in the injection site, <em>longissimus dorsi</em> muscle, liver or kidney samples collected from the goats. The reported analytical method and residue depletion data provide a foundation for future thiafentanil and naltrexone residue depletion studies in wildlife species.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"257 ","pages":"Article 116711"},"PeriodicalIF":3.1,"publicationDate":"2025-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143161410","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

The nonanol/surfactant directed self-assembly supramoleculars heat-shrinkable tubing liquid phase microextraction for determination of flavonoids in natural products combined with high performance liquid chromatography

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-01-30 DOI: 10.1016/j.jpba.2025.116704

Jie Li , Weizheng Fu , Yuzhen Zhang , Shuang Hu , Xuan Chen

In this paper, a supramolecular heat-shrinkable tubing liquid phase microextraction was developed for the enrichment and determination of flavonoids. The nonanol adsorbed by the heat-shrinkable tubing could induce the surfactant in aqueous solution to self-assembly on its surface, and formed nonanol/CTAB supramolecules in a directional arrangement. The supramolecules structure enhanced the enrichment efficiency of five flavonoids. The parameters affecting the extraction efficiency were optimized, such as the type of organic solvent, concentration of surfactant, pH and volume of sample phase, salt concentration of sample solution, stirring speed and extraction time. The methodological investigation was carried out under the optimal experimental conditions. The enrichment factors of the five analytes were between 72.3 and 93.3. The concentrations of the target analytes showed good linearity between 0.2 and 5 µg/mL, 0.01–1 µg/mL, 0.01–5 µg/mL, respectively. The limit of detection was no more than 25 ng/mL. The procedure was successfully applied in extraction of five flavonoids from the natural products according to its average recoveries of 98.3–101.7 %.

{"title":"The nonanol/surfactant directed self-assembly supramoleculars heat-shrinkable tubing liquid phase microextraction for determination of flavonoids in natural products combined with high performance liquid chromatography","authors":"Jie Li , Weizheng Fu , Yuzhen Zhang , Shuang Hu , Xuan Chen","doi":"10.1016/j.jpba.2025.116704","DOIUrl":"10.1016/j.jpba.2025.116704","url":null,"abstract":"<div><div>In this paper, a supramolecular heat-shrinkable tubing liquid phase microextraction was developed for the enrichment and determination of flavonoids. The nonanol adsorbed by the heat-shrinkable tubing could induce the surfactant in aqueous solution to self-assembly on its surface, and formed nonanol/CTAB supramolecules in a directional arrangement. The supramolecules structure enhanced the enrichment efficiency of five flavonoids. The parameters affecting the extraction efficiency were optimized, such as the type of organic solvent, concentration of surfactant, pH and volume of sample phase, salt concentration of sample solution, stirring speed and extraction time. The methodological investigation was carried out under the optimal experimental conditions. The enrichment factors of the five analytes were between 72.3 and 93.3. The concentrations of the target analytes showed good linearity between 0.2 and 5 µg/mL, 0.01–1 µg/mL, 0.01–5 µg/mL, respectively. The limit of detection was no more than 25 ng/mL. The procedure was successfully applied in extraction of five flavonoids from the natural products according to its average recoveries of 98.3–101.7 %.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"258 ","pages":"Article 116704"},"PeriodicalIF":3.1,"publicationDate":"2025-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143180465","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

A strategy integrated DNA barcoding with metabolomics for screening distinguishable combinatorial chemical quality marker between Pheretima aspergillum and Pheretima vulgaris Chen

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-01-29 DOI: 10.1016/j.jpba.2025.116716

Ye Shang , Suyi Liu , Chunxiao Liang , Tenukeguli Tuliebieke , Shujing Chen , Kunze Du , Xiaoxuan Tian , Jin Li , Jun He , Hua Jin , Yanxu Chang

Pheretima is an animal-derived traditional Chinese medicines (TCMs). The chemical quality markers of Pheretima used to distinguish different species are still ambiguous. Under this premise, a strategy integrated DNA barcoding with metabolomics is promoted for identifying Pheretima and screening distinguishable combinatorial chemical quality marker (DCQ-marker) between Pheretima aspergillum (P. aspergillum) and Pheretima vulgaris Chen (P. vulgaris). As a result, adenosine, adenine, L-phenylalanine and uridine are successfully selected as DCQ-markers between P. aspergillum and P. vulgaris. This study provides convenient strategy for quickly screening DCQ-marker between P. aspergillum and P. vulgaris. It will be meaningful for further promoting quality control on Pheretima and providing a reference for the quality evaluation of other animal-derived TCMs.

{"title":"A strategy integrated DNA barcoding with metabolomics for screening distinguishable combinatorial chemical quality marker between Pheretima aspergillum and Pheretima vulgaris Chen","authors":"Ye Shang , Suyi Liu , Chunxiao Liang , Tenukeguli Tuliebieke , Shujing Chen , Kunze Du , Xiaoxuan Tian , Jin Li , Jun He , Hua Jin , Yanxu Chang","doi":"10.1016/j.jpba.2025.116716","DOIUrl":"10.1016/j.jpba.2025.116716","url":null,"abstract":"<div><div><em>Pheretima</em> is an animal-derived traditional Chinese medicines (TCMs). The chemical quality markers of <em>Pheretima</em> used to distinguish different species are still ambiguous. Under this premise, a strategy integrated DNA barcoding with metabolomics is promoted for identifying <em>Pheretima</em> and screening distinguishable combinatorial chemical quality marker (DCQ-marker) between <em>Pheretima aspergillum</em> (<em>P. aspergillum</em>) and <em>Pheretima vulgaris</em> Chen (<em>P. vulgaris</em>). As a result, adenosine, adenine, L-phenylalanine and uridine are successfully selected as DCQ-markers between <em>P. aspergillum</em> and <em>P. vulgaris</em>. This study provides convenient strategy for quickly screening DCQ-marker between <em>P. aspergillum</em> and <em>P. vulgaris</em>. It will be meaningful for further promoting quality control on <em>Pheretima</em> and providing a reference for the quality evaluation of other animal-derived TCMs.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"257 ","pages":"Article 116716"},"PeriodicalIF":3.1,"publicationDate":"2025-01-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143080264","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

Monolithic and hierarchically porous biochar/cellulose aerogel as adsorbent for microextraction in packed syringe towards trace sulfonamides in water samples prior to UPLC-MS/MS

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-01-29 DOI: 10.1016/j.jpba.2025.116714

Sai Li, Shuangying Yu, Mengyao Zhang, Zeyi Li, Hui Yu, Zhongfu Xing, Beibei Mao, Pan Zhao

In this study, biochars with desirable adsorption capacity were prepared by calcination of herbal medicine residue, and the obtained biochars were loaded on cellulose aerogel through a green synthesis method. The monolithic biochar/cellulose aerogel hybrid was packed in the syringe and used as adsorbent for microextraction in packed syringe (MEPS). After introducing cellulose aerogel as the support, the loss of powdered biochars was avoided, and the entire extraction process can be achieved through simple operation of filtration due to the macroporous structure of cellulose aerogel. Coupled with UPLC-MS/MS, the established method was successfully applied to determine trace level of sulfonamides (SAs) in water samples. Extraction parameters such as pH of sample solution, adsorbent type, sample volume, elution solvent type and elution solvent volume were studied. Under the optimized parameters (pH of sample solution:7, adsorbent type: biochar/cellulose aerogel, sample volume: 20 mL, elution solvent: 0.3 mL methanol, the number of aspiration and dispense of sample solution, washing solvent and elution solvent: 3), desirable linearity correlation coefficient (r) in the range of 0.9951–0.9972 was achieved. The limit of detection varied from 0.00407 to 0.0104 ng/mL, and recovery ranging from 65.3 % to 102.4 % was obtained. The proposed method was demonstrated to be sensitive, accurate and easily operative, providing a convenient protocol for sample pretreatment.

{"title":"Monolithic and hierarchically porous biochar/cellulose aerogel as adsorbent for microextraction in packed syringe towards trace sulfonamides in water samples prior to UPLC-MS/MS","authors":"Sai Li, Shuangying Yu, Mengyao Zhang, Zeyi Li, Hui Yu, Zhongfu Xing, Beibei Mao, Pan Zhao","doi":"10.1016/j.jpba.2025.116714","DOIUrl":"10.1016/j.jpba.2025.116714","url":null,"abstract":"<div><div>In this study, biochars with desirable adsorption capacity were prepared by calcination of herbal medicine residue, and the obtained biochars were loaded on cellulose aerogel through a green synthesis method. The monolithic biochar/cellulose aerogel hybrid was packed in the syringe and used as adsorbent for microextraction in packed syringe (MEPS). After introducing cellulose aerogel as the support, the loss of powdered biochars was avoided, and the entire extraction process can be achieved through simple operation of filtration due to the macroporous structure of cellulose aerogel. Coupled with UPLC-MS/MS, the established method was successfully applied to determine trace level of sulfonamides (SAs) in water samples. Extraction parameters such as pH of sample solution, adsorbent type, sample volume, elution solvent type and elution solvent volume were studied. Under the optimized parameters (pH of sample solution:7, adsorbent type: biochar/cellulose aerogel, sample volume: 20 mL, elution solvent: 0.3 mL methanol, the number of aspiration and dispense of sample solution, washing solvent and elution solvent: 3), desirable linearity correlation coefficient (r) in the range of 0.9951–0.9972 was achieved. The limit of detection varied from 0.00407 to 0.0104 ng/mL, and recovery ranging from 65.3 % to 102.4 % was obtained. The proposed method was demonstrated to be sensitive, accurate and easily operative, providing a convenient protocol for sample pretreatment.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"257 ","pages":"Article 116714"},"PeriodicalIF":3.1,"publicationDate":"2025-01-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143080267","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

Quantification of amino acids in small volumes of human sweat collected from fingertips of healthy subjects at rest

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-01-29 DOI: 10.1016/j.jpba.2025.116718

Hiroshi Kuroki, Makoto Tsunoda

Sweat is a body fluid that can be collected noninvasively. Sweat can be utilized as a biofluid for quantification of amino acids for clinical applications, such as disease screening. Amino acids are essential for many biological processes in the human body. Hence, the development of analytical methods for determining the concentrations of amino acids in human sweat can offer valuable insights into the health status of an individual. Sweat analysis can further be utilized as a tool for screening various pathological conditions. In this study, the concentrations of amino acids in small volumes of human sweat collected from fingertips of healthy subjects at rest were investigated. Reliable sweat collection was achieved by optimizing the sample collection procedure. The amino acids in human sweat were derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole, followed by analysis using high-performance liquid chromatography with fluorescence detection. The amino acid concentrations in sweat were quantified. The temporal variability and sex-specific differences in the concentrations of amino acids were evaluated. The results of both intra- and inter-day sweat analyses revealed that except for citrulline and arginine, the concentrations of other amino acids in sweat are relatively stable. This study proposes that the concentrations of amino acids in sweat can be determined with high accuracy, regardless of sweat collection timing. The findings of this study provide useful information that can help develop disease screening methods based on sweat analysis.

{"title":"Quantification of amino acids in small volumes of human sweat collected from fingertips of healthy subjects at rest","authors":"Hiroshi Kuroki, Makoto Tsunoda","doi":"10.1016/j.jpba.2025.116718","DOIUrl":"10.1016/j.jpba.2025.116718","url":null,"abstract":"<div><div>Sweat is a body fluid that can be collected noninvasively. Sweat can be utilized as a biofluid for quantification of amino acids for clinical applications, such as disease screening. Amino acids are essential for many biological processes in the human body. Hence, the development of analytical methods for determining the concentrations of amino acids in human sweat can offer valuable insights into the health status of an individual. Sweat analysis can further be utilized as a tool for screening various pathological conditions. In this study, the concentrations of amino acids in small volumes of human sweat collected from fingertips of healthy subjects at rest were investigated. Reliable sweat collection was achieved by optimizing the sample collection procedure. The amino acids in human sweat were derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole, followed by analysis using high-performance liquid chromatography with fluorescence detection. The amino acid concentrations in sweat were quantified. The temporal variability and sex-specific differences in the concentrations of amino acids were evaluated. The results of both intra- and inter-day sweat analyses revealed that except for citrulline and arginine, the concentrations of other amino acids in sweat are relatively stable. This study proposes that the concentrations of amino acids in sweat can be determined with high accuracy, regardless of sweat collection timing. The findings of this study provide useful information that can help develop disease screening methods based on sweat analysis.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"257 ","pages":"Article 116718"},"PeriodicalIF":3.1,"publicationDate":"2025-01-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143161413","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Molecular mass spectrometric imaging of amino acids in dietary supplement tablets using laser ablation-atmospheric pressure chemical ionization-trapped ion mobility spectrometry-mass spectrometry

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-01-29 DOI: 10.1016/j.jpba.2025.116719

Johannes Schmeinck, Uwe Karst

A UV laser ablation system coupled to atmospheric pressure chemical ionization-trapped ion mobility spectrometry-mass spectrometry (LA-APCI-TIMS-MS) is presented as a novel mass spectrometry imaging (MSI) tool to investigate the distribution of amino acids and vitamins in dietary supplement tablets. The setup employs a custom-built LA interface for commercially available APCI sources. Average single pulse response (SPR) durations of less than 0.2 s full peak width at 1 % maximum (FW0.01 M) were achieved. Imaging analyses resulted in the detection of 16 amino acids and 10 vitamins, all with unique and complementary distributions that are in most cases heterogeneously distributed over the sample surface. To differentiate between leucine and isoleucine, a second analysis was conducted on the same amino acid tablet with TIMS, showing distinct distributions for the two compounds. These results illustrate the potential of the presented setup to gain insight into the composition and manufacturing conditions of dietary supplements.

{"title":"Molecular mass spectrometric imaging of amino acids in dietary supplement tablets using laser ablation-atmospheric pressure chemical ionization-trapped ion mobility spectrometry-mass spectrometry","authors":"Johannes Schmeinck, Uwe Karst","doi":"10.1016/j.jpba.2025.116719","DOIUrl":"10.1016/j.jpba.2025.116719","url":null,"abstract":"<div><div>A UV laser ablation system coupled to atmospheric pressure chemical ionization-trapped ion mobility spectrometry-mass spectrometry (LA-APCI-TIMS-MS) is presented as a novel mass spectrometry imaging (MSI) tool to investigate the distribution of amino acids and vitamins in dietary supplement tablets. The setup employs a custom-built LA interface for commercially available APCI sources. Average single pulse response (SPR) durations of less than 0.2 s full peak width at 1 % maximum (FW0.01 M) were achieved. Imaging analyses resulted in the detection of 16 amino acids and 10 vitamins, all with unique and complementary distributions that are in most cases heterogeneously distributed over the sample surface. To differentiate between leucine and isoleucine, a second analysis was conducted on the same amino acid tablet with TIMS, showing distinct distributions for the two compounds. These results illustrate the potential of the presented setup to gain insight into the composition and manufacturing conditions of dietary supplements.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"257 ","pages":"Article 116719"},"PeriodicalIF":3.1,"publicationDate":"2025-01-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143074835","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Immunomagnetic bead-based sample preparation method and immunoassay for detecting higenamine in herbal products

IF 3.1 3区医学 Q2 CHEMISTRY, ANALYTICAL

Journal of pharmaceutical and biomedical analysis

Pub Date : 2025-01-28 DOI: 10.1016/j.jpba.2025.116712

Jinping Qiu, Rui Zhang, Wentao Liu, Yang Lu, Jifeng Liu

Higenamine (HM), classified as an S3 β2 agonist and prohibited by the World Anti-Doping Agency (WADA), is prevalent in spices and traditional Chinese herbal medicines.Accidental consumption can lead to HM positivity in athletes, necessitating daily monitoring. However, current detection strategies predominantly involve instrumental analysis, with limited development of rapid methodologies incorporating sample preparation for practical, daily applications. In this study, a novel method has been developed for the rapid and quantitative detection of HM in throat lozenges, plant beverages, syrups and grass coral. This innovative approach combines the use of immunomagnetic beads and an indirect competitive enzyme-linked immunosorbent assay (ic-ELISA) to achieve efficient enrichment and detection. In the assay development, a highly sensitive anti-HM monoclonal antibody 1E9 (1E9-mAb) was generated and its binding mechanism to HM was investigated by theoretical simulations. Under optimum conditions, the sensitivity (IC₅₀) and detection limit (IC₁₅) were 0.23 ± 0.02 ng/mL and 0.04 ± 0.01 ng/mL. The detection limits for throat lozenges, plant beverages and syrups were 3, 4, and 2 μg/kg, respectively. The developed assay has been used to detect HM in 28 products on the market. This is the first HM detection method with immunomagnetic beads for sample preparation, and HM was found in grass coral extract and its processed products for the first time. Compared with the previous methods, it provides a more simple and efficient method of detecting trace HM in food and medicines daily.

{"title":"Immunomagnetic bead-based sample preparation method and immunoassay for detecting higenamine in herbal products","authors":"Jinping Qiu, Rui Zhang, Wentao Liu, Yang Lu, Jifeng Liu","doi":"10.1016/j.jpba.2025.116712","DOIUrl":"10.1016/j.jpba.2025.116712","url":null,"abstract":"<div><div>Higenamine (HM), classified as an S3 β2 agonist and prohibited by the World Anti-Doping Agency (WADA), is prevalent in spices and traditional Chinese herbal medicines.Accidental consumption can lead to HM positivity in athletes, necessitating daily monitoring. However, current detection strategies predominantly involve instrumental analysis, with limited development of rapid methodologies incorporating sample preparation for practical, daily applications. In this study, a novel method has been developed for the rapid and quantitative detection of HM in throat lozenges, plant beverages, syrups and grass coral. This innovative approach combines the use of immunomagnetic beads and an indirect competitive enzyme-linked immunosorbent assay (ic-ELISA) to achieve efficient enrichment and detection. In the assay development, a highly sensitive anti-HM monoclonal antibody 1E9 (1E9-mAb) was generated and its binding mechanism to HM was investigated by theoretical simulations. Under optimum conditions, the sensitivity (IC<sub>50</sub>) and detection limit (IC<sub>15</sub>) were 0.23 ± 0.02 ng/mL and 0.04 ± 0.01 ng/mL. The detection limits for throat lozenges, plant beverages and syrups were 3, 4, and 2 μg/kg, respectively. The developed assay has been used to detect HM in 28 products on the market. This is the first HM detection method with immunomagnetic beads for sample preparation, and HM was found in grass coral extract and its processed products for the first time. Compared with the previous methods, it provides a more simple and efficient method of detecting trace HM in food and medicines daily.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"257 ","pages":"Article 116712"},"PeriodicalIF":3.1,"publicationDate":"2025-01-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143074834","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}

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