Baoxin Xu, Weiwei Zhou, Yanrong Li, Shengnan Zhao, Yilong Du, Xia Hong, Haifeng Pan, Chenfeng Wang
In this study, a rapid and sensitive ultra‐high performance liquid chromatography‐tandem mass spectrometry method was established for the simultaneous determination of four Vitexin‐4“‐O‐glucoside (VOG), Vitexin‐2”‐O‐rhamnoside (VOR), vitexin (VIT), and hyperoside (HP) in plasma, which are representative flavonoids constituents of hawthorn leaves. The four components were separated by CORTECS UPLC C18 column (100 × 3.0 mm, 1.6 µm), using acetonitrile‐water containing 0.02% formic acid and 2 mmol/L ammonium formate as the mobile phase, the gradient elution flow rate was 0.30 mL/min. The analyte was quantified using an electrospray ionization triple quadrupole mass spectrometer. The analytes and baicalin internal standard were performed at m/z 593.2/413.2 for VOG, m/z 577.2/413.1 for VOR, m/z 431.1/310.9 for VIT, m/z 463.2/300 for HP and m/z 445.1/269 for internal standard. Among the four flavonoids, the correlation coefficient of the standard curve of each component is between 0.9939 and 0.9987. After oral administration of hawthorn leaf extract, VOG and VOR showed similar pharmacokinetic characteristics; VIT was eliminated in the body more slowly than the other three flavonoids and distributed more in the tissues; HP can be quickly absorbed in the blood. The developed analytical method has high sensitivity, precision, and accuracy with no interference from plasma components and has been successfully used in pharmacokinetic studies.
{"title":"Rapid determination of four flavonoids from hawthorn leaves in plasma by ultra‐high performance liquid chromatography‐tandem mass spectrometry and study on its pharmacokinetics","authors":"Baoxin Xu, Weiwei Zhou, Yanrong Li, Shengnan Zhao, Yilong Du, Xia Hong, Haifeng Pan, Chenfeng Wang","doi":"10.1002/sscp.202300221","DOIUrl":"https://doi.org/10.1002/sscp.202300221","url":null,"abstract":"In this study, a rapid and sensitive ultra‐high performance liquid chromatography‐tandem mass spectrometry method was established for the simultaneous determination of four Vitexin‐4“‐O‐glucoside (VOG), Vitexin‐2”‐O‐rhamnoside (VOR), vitexin (VIT), and hyperoside (HP) in plasma, which are representative flavonoids constituents of hawthorn leaves. The four components were separated by CORTECS UPLC C18 column (100 × 3.0 mm, 1.6 µm), using acetonitrile‐water containing 0.02% formic acid and 2 mmol/L ammonium formate as the mobile phase, the gradient elution flow rate was 0.30 mL/min. The analyte was quantified using an electrospray ionization triple quadrupole mass spectrometer. The analytes and baicalin internal standard were performed at m/z 593.2/413.2 for VOG, m/z 577.2/413.1 for VOR, m/z 431.1/310.9 for VIT, m/z 463.2/300 for HP and m/z 445.1/269 for internal standard. Among the four flavonoids, the correlation coefficient of the standard curve of each component is between 0.9939 and 0.9987. After oral administration of hawthorn leaf extract, VOG and VOR showed similar pharmacokinetic characteristics; VIT was eliminated in the body more slowly than the other three flavonoids and distributed more in the tissues; HP can be quickly absorbed in the blood. The developed analytical method has high sensitivity, precision, and accuracy with no interference from plasma components and has been successfully used in pharmacokinetic studies.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141099953","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Hongwei Song, Hui Sun, Heng Fang, Le Yang, Qiqi Zhao, Ye Sun, Guang-li Yan, Ying Han, Xijun Wang
Hirudo is a medicinal and edible homologous animal. Its rich polypeptides have been proven to have strong biological activity and effects on human health or disease. However, the quality control of hirudo can still be improved. Based on the traditional scientific understanding of oral hirudo administration, this study adopted artificial gastric‐juice extraction combined with pepsin enzymolysis to simulate the digestion and absorption of gastrointestinal tract after taking hirudo. Ultrahigh‐performance liquid chromatography–mass spectrometry technology was initially used to screen and characterize 52 enzymolysis components of hirudo. The fingerprint of hirudo enzymolysis polypeptide was then established. The method was confirmed to have high accuracy, repeatability, and stability. Using the established hirudo enzymolysis polypeptide fingerprint, we proved that it can effectively identify different origins of hirudo. The established fingerprint revealed that 19 enzymolysis polypeptides derived from hirudo in the Qizhi capsule, indicating that it can promote and improve the quality control of Qizhi capsule. The present study provided a new technology and idea for the origin identification and quality control of hirudo, and standards for Chinese patent medicines containing hirudo. It can also serve as a reference for the quality control of other animal‐origin drugs or foods.
{"title":"Fingerprint profile analysis of hirudo polypeptide based on UHPLC–MS and its application","authors":"Hongwei Song, Hui Sun, Heng Fang, Le Yang, Qiqi Zhao, Ye Sun, Guang-li Yan, Ying Han, Xijun Wang","doi":"10.1002/sscp.202300218","DOIUrl":"https://doi.org/10.1002/sscp.202300218","url":null,"abstract":"Hirudo is a medicinal and edible homologous animal. Its rich polypeptides have been proven to have strong biological activity and effects on human health or disease. However, the quality control of hirudo can still be improved. Based on the traditional scientific understanding of oral hirudo administration, this study adopted artificial gastric‐juice extraction combined with pepsin enzymolysis to simulate the digestion and absorption of gastrointestinal tract after taking hirudo. Ultrahigh‐performance liquid chromatography–mass spectrometry technology was initially used to screen and characterize 52 enzymolysis components of hirudo. The fingerprint of hirudo enzymolysis polypeptide was then established. The method was confirmed to have high accuracy, repeatability, and stability. Using the established hirudo enzymolysis polypeptide fingerprint, we proved that it can effectively identify different origins of hirudo. The established fingerprint revealed that 19 enzymolysis polypeptides derived from hirudo in the Qizhi capsule, indicating that it can promote and improve the quality control of Qizhi capsule. The present study provided a new technology and idea for the origin identification and quality control of hirudo, and standards for Chinese patent medicines containing hirudo. It can also serve as a reference for the quality control of other animal‐origin drugs or foods.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141121839","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Marios C. Christodoulou, Diego J. Gonzalez‐Serrano, A. Christou, Ioannis J. Stavrou, Milad Hadidi, Andres Moreno, Constantina P. Kapnissi‐Christodoulou
Microwave‐assisted extraction (MAE) of cannabinoids from hemp tea was optimized, for the first, using response surface methodology. The effect of temperature (50, 65, and 80°C), irradiation time (4, 7, and 10 min), and solvent‐to‐solid ratio (20, 30, and 40 mL of methanol/g of hemp tea) on cannabinoid extractability were investigated. The concentrations of five cannabinoids, namely Δ9‐tetrahydrocannabinol (Δ9‐THC), cannabidiol (CBD), cannabigerol (CBG), cannabichromene (CBC), and cannabinol (CBN), were selected as response variables. For the quantitative analysis, a liquid chromatography‐mass spectrometry method was developed and validated. The proposed analytical approach demonstrated satisfactory performance characteristics in terms of linearity (R2 ≥ 0.9998), precision (intra‐day: 1.99%–5.97% relative standard deviation [%RSD], inter‐day: 1.95%–6.08%RSD), sensitivity (limit of detection: 1.35–2.36 ng/g, limit of quantification: 4.05–7.08 ng/g) and carry‐over effect (signals ≤ 5.03%), with all cannabinoids eluting within 6 min. For comparison purposes, soxhlet extraction, ultrasound‐assisted extraction (UAE), and conventional‐stirring extraction were additionally performed. MAE proved to be a more effective technique for the extraction of CBD and CBN, while UAE managed to extract Δ9‐THC, CBG, and CBC at higher concentration levels.
{"title":"Optimization of microwave‐assisted extraction for quantification of cannabinoids in hemp tea by liquid chromatography‐mass spectrometry","authors":"Marios C. Christodoulou, Diego J. Gonzalez‐Serrano, A. Christou, Ioannis J. Stavrou, Milad Hadidi, Andres Moreno, Constantina P. Kapnissi‐Christodoulou","doi":"10.1002/sscp.202300220","DOIUrl":"https://doi.org/10.1002/sscp.202300220","url":null,"abstract":"Microwave‐assisted extraction (MAE) of cannabinoids from hemp tea was optimized, for the first, using response surface methodology. The effect of temperature (50, 65, and 80°C), irradiation time (4, 7, and 10 min), and solvent‐to‐solid ratio (20, 30, and 40 mL of methanol/g of hemp tea) on cannabinoid extractability were investigated. The concentrations of five cannabinoids, namely Δ9‐tetrahydrocannabinol (Δ9‐THC), cannabidiol (CBD), cannabigerol (CBG), cannabichromene (CBC), and cannabinol (CBN), were selected as response variables. For the quantitative analysis, a liquid chromatography‐mass spectrometry method was developed and validated. The proposed analytical approach demonstrated satisfactory performance characteristics in terms of linearity (R2 ≥ 0.9998), precision (intra‐day: 1.99%–5.97% relative standard deviation [%RSD], inter‐day: 1.95%–6.08%RSD), sensitivity (limit of detection: 1.35–2.36 ng/g, limit of quantification: 4.05–7.08 ng/g) and carry‐over effect (signals ≤ 5.03%), with all cannabinoids eluting within 6 min. For comparison purposes, soxhlet extraction, ultrasound‐assisted extraction (UAE), and conventional‐stirring extraction were additionally performed. MAE proved to be a more effective technique for the extraction of CBD and CBN, while UAE managed to extract Δ9‐THC, CBG, and CBC at higher concentration levels.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140969207","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Tainara Guizolfi, Airton Kramer, Rafael Menck, S. Moura
Amphetamines (AMPHs) and their derivatives are potent central nervous system stimulants, in 2020 an astonishing 34 million regular users were reported worldwide. Consequently, there has been a critical need for the development of methods capable of detecting these compounds in alternative biological matrices. The review article discusses the analysis of amphetamines and their derivatives in alternative biological matrices, such as hair and oral fluid (OF), using liquid chromatography‐mass spectrometry. Compiles data from 28 articles published between 2012 and 2022, focusing on 13 articles on OFs and 15 on hair analysis. The article highlights the advantages of using these alternative matrices, including less invasive collection methods, greater sample stability, and simplified extraction processes. Additionally, prevalent analytical practices such as the use of C18 columns and the incorporation of formic acid and methanol into mobile phases are discussed. Furthermore, it demonstrates that the most used method for collecting OF is the Quantisal device, as well as solid phase extraction is also the most used for the same matrix. The review serves as a guide for researchers interested in analytical methods for identifying AMPHs, offering insights into advances, challenges, and the most used in the area.
{"title":"Advancements in liquid chromatography‐mass spectrometry for amphetamine analysis in unconventional biological matrices: Focus on oral fluid and hair samples","authors":"Tainara Guizolfi, Airton Kramer, Rafael Menck, S. Moura","doi":"10.1002/sscp.202400019","DOIUrl":"https://doi.org/10.1002/sscp.202400019","url":null,"abstract":"Amphetamines (AMPHs) and their derivatives are potent central nervous system stimulants, in 2020 an astonishing 34 million regular users were reported worldwide. Consequently, there has been a critical need for the development of methods capable of detecting these compounds in alternative biological matrices. The review article discusses the analysis of amphetamines and their derivatives in alternative biological matrices, such as hair and oral fluid (OF), using liquid chromatography‐mass spectrometry. Compiles data from 28 articles published between 2012 and 2022, focusing on 13 articles on OFs and 15 on hair analysis. The article highlights the advantages of using these alternative matrices, including less invasive collection methods, greater sample stability, and simplified extraction processes. Additionally, prevalent analytical practices such as the use of C18 columns and the incorporation of formic acid and methanol into mobile phases are discussed. Furthermore, it demonstrates that the most used method for collecting OF is the Quantisal device, as well as solid phase extraction is also the most used for the same matrix. The review serves as a guide for researchers interested in analytical methods for identifying AMPHs, offering insights into advances, challenges, and the most used in the area.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140993790","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Duan Yu, Zhongjing Guo, Zhimin Zhao, Yang Depo, xinjun Xu
In this paper, a simple and efficient high‐performance liquid chromatography method was established to analyze the chemical composition fingerprint of Centellae Herba (CHA) and determine five triterpenoid active components in CHA, namely, asiaticoside B (AB), madecassoside, asiaticoside, madecasic acid, and asiaticoic acid. The separation of the compounds was carried out on an XD‐C18 column (250 mm × 4.6 mm, 5 µm), the wavelength of the ultraviolet detector was set to 205 nm, and the mobile phase was composed of acetonitrile −0.05% phosphoric acid, 2 mmol/L β‐cyclodextrin aqueous solution, and gradient elution at the flow rate of 1.0 mL/min. A general chromatographic fingerprint consisting of 20 characteristic peaks of 18 batches of CHA samples was established, and the samples were classified and evaluated by similarity analysis, hierarchical cluster analysis, and principal component analysis combined with multivariate econometric analysis. In quantitative analysis, all calibration curves showed good linear regression in the test range (r > 0.999), the average recovery was 96.12%–104.63%, and the relative standard deviations of repeatability and stability were less than 2.00%. The results show that the method is accurate and effective and can be used for the comprehensive quality control of CHA.
本文建立了一种简便高效的高效液相色谱法,用于分析积雪草的化学成分指纹图谱,并测定了积雪草中的5种三萜类活性成分,即积雪草苷B(AB)、积雪草苷、积雪草苷、积雪草酸和积雪草酸。采用XD-C18色谱柱（250 mm × 4.6 mm, 5 µm）进行分离，紫外检测器波长为205 nm，流动相为乙腈-0.05%磷酸、2 mmol/Lβ-环糊精水溶液，梯度洗脱，流速为1.0 mL/min。建立了由 18 批 CHA 样品的 20 个特征峰组成的通用色谱指纹图谱，并通过相似性分析、层次聚类分析和主成分分析结合多元计量经济学分析对样品进行了分类和评价。定量分析结果表明，所有定标曲线在检测范围内线性回归良好（r>0.999），平均回收率为96.12%～104.63%，重复性和稳定性的相对标准偏差均小于2.00%。结果表明该方法准确、有效，可用于CHA的全面质量控制。
{"title":"Establishment of chemical fingerprint and determination of main active ingredients in Centellae Herba by HPLC combined with multivariate chemometrics analysis","authors":"Duan Yu, Zhongjing Guo, Zhimin Zhao, Yang Depo, xinjun Xu","doi":"10.1002/sscp.202400021","DOIUrl":"https://doi.org/10.1002/sscp.202400021","url":null,"abstract":"In this paper, a simple and efficient high‐performance liquid chromatography method was established to analyze the chemical composition fingerprint of Centellae Herba (CHA) and determine five triterpenoid active components in CHA, namely, asiaticoside B (AB), madecassoside, asiaticoside, madecasic acid, and asiaticoic acid. The separation of the compounds was carried out on an XD‐C18 column (250 mm × 4.6 mm, 5 µm), the wavelength of the ultraviolet detector was set to 205 nm, and the mobile phase was composed of acetonitrile −0.05% phosphoric acid, 2 mmol/L β‐cyclodextrin aqueous solution, and gradient elution at the flow rate of 1.0 mL/min. A general chromatographic fingerprint consisting of 20 characteristic peaks of 18 batches of CHA samples was established, and the samples were classified and evaluated by similarity analysis, hierarchical cluster analysis, and principal component analysis combined with multivariate econometric analysis. In quantitative analysis, all calibration curves showed good linear regression in the test range (r > 0.999), the average recovery was 96.12%–104.63%, and the relative standard deviations of repeatability and stability were less than 2.00%. The results show that the method is accurate and effective and can be used for the comprehensive quality control of CHA.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140991114","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Rhododendron petals are considered high‐value owing to their commercial utility, national/state flower status in certain countries, and bioactive potential from recent studies. Profiling and quantitative analysis of the bioactive metabolites would evaluate if they can be natural sources. This study is focused on the comprehensive profiling of secondary metabolites in the hot aqueous petal extracts of Red and Pink Rhododendron flowers (Rhododendron arboreum and Rhododendron campanulatum) using separation and fragmentation patterns from mass spectrometry (MS) (gas chromatography‐MS and liquid chromatography‐tandem MS) and chemical shifts from proton‐nuclear magnetic resonance spectroscopy. The complementary analytical platforms highlighted the petals to be rich in promising bioactive molecules such as quinic acid, chlorogenic acid (caffeoyl quinic acid), protocatechuic acid, coumaroyl quinic acids, catechin, epigallocatechin, and shikimic acid. The analysis also reflected the activity of shikimic acid, phenolic acid, and flavonoid biosynthetic pathways in Rhododendron flowers. These metabolites are well reported for their bioactive potential as anti‐oxidative, anti‐viral, anti‐cancerous, anti‐diabetic, anti‐inflammatory, etc. While the quantitative and multivariate analysis showed variations in the levels of phenolic acids and flavonoids, it is established that red and pink Rhododendron flower petals are a rich source of bioactive phytochemicals of interest to the phytochemical Industry.
{"title":"Mass spectrometry and Nuclear magnetic resonance spectroscopy profiles of red and pink Rhododendron flower petals establish them as rich sources of bioactive secondary metabolites","authors":"S. Shagun, Maneesh Lingwan, S. K. Masakapalli","doi":"10.1002/sscp.202400007","DOIUrl":"https://doi.org/10.1002/sscp.202400007","url":null,"abstract":"Rhododendron petals are considered high‐value owing to their commercial utility, national/state flower status in certain countries, and bioactive potential from recent studies. Profiling and quantitative analysis of the bioactive metabolites would evaluate if they can be natural sources. This study is focused on the comprehensive profiling of secondary metabolites in the hot aqueous petal extracts of Red and Pink Rhododendron flowers (Rhododendron arboreum and Rhododendron campanulatum) using separation and fragmentation patterns from mass spectrometry (MS) (gas chromatography‐MS and liquid chromatography‐tandem MS) and chemical shifts from proton‐nuclear magnetic resonance spectroscopy. The complementary analytical platforms highlighted the petals to be rich in promising bioactive molecules such as quinic acid, chlorogenic acid (caffeoyl quinic acid), protocatechuic acid, coumaroyl quinic acids, catechin, epigallocatechin, and shikimic acid. The analysis also reflected the activity of shikimic acid, phenolic acid, and flavonoid biosynthetic pathways in Rhododendron flowers. These metabolites are well reported for their bioactive potential as anti‐oxidative, anti‐viral, anti‐cancerous, anti‐diabetic, anti‐inflammatory, etc. While the quantitative and multivariate analysis showed variations in the levels of phenolic acids and flavonoids, it is established that red and pink Rhododendron flower petals are a rich source of bioactive phytochemicals of interest to the phytochemical Industry.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140993944","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Golnaz Golmohammadi, H. Sereshti, S. Samadi, H. Rashidi Nodeh
Catechins, as powerful flavonoids with antioxidant properties, are crucial for the preservation of the human body against free radicals and for promoting overall health. Research has shown that the presence of catechins in urine is linked to a reduced risk of gastric and esophageal cancer. This study introduces an innovative approach using a novel nano‐composite material, composed of magnetic graphene oxide coated with a biocompatible O‐carboxymethyl chitosan/acrylic acid copolymer, for extracting catechins from human urine. The extracted catechins were then analyzed using gas chromatography/mass spectrometry‐selected ion monitoring analysis. Under the optimum conditions, the analytical figures of merit for catechin and epicatechin were linear dynamic range: 0.5–1000 ng/mL, R2 of 0.9991; limit of detection equal to 0.1 ng/mL; relative standard deviation: 4.1 and 3.1 (C = 50 ng/mL, n = 3); and relative recovery was 94%, respectively. The application of this method holds significant promise for advancing clinical and toxicological studies, as well as establishing potential associations between tea consumption and disease prevention.
{"title":"A biocompatible O‐carboxymethyl chitosan/acrylic acid copolymer over magnetic graphene oxide used for determination of catechins in urine prior to ion monitoring‐gas chromatography/mass spectrometry","authors":"Golnaz Golmohammadi, H. Sereshti, S. Samadi, H. Rashidi Nodeh","doi":"10.1002/sscp.202300151","DOIUrl":"https://doi.org/10.1002/sscp.202300151","url":null,"abstract":"Catechins, as powerful flavonoids with antioxidant properties, are crucial for the preservation of the human body against free radicals and for promoting overall health. Research has shown that the presence of catechins in urine is linked to a reduced risk of gastric and esophageal cancer. This study introduces an innovative approach using a novel nano‐composite material, composed of magnetic graphene oxide coated with a biocompatible O‐carboxymethyl chitosan/acrylic acid copolymer, for extracting catechins from human urine. The extracted catechins were then analyzed using gas chromatography/mass spectrometry‐selected ion monitoring analysis. Under the optimum conditions, the analytical figures of merit for catechin and epicatechin were linear dynamic range: 0.5–1000 ng/mL, R2 of 0.9991; limit of detection equal to 0.1 ng/mL; relative standard deviation: 4.1 and 3.1 (C = 50 ng/mL, n = 3); and relative recovery was 94%, respectively. The application of this method holds significant promise for advancing clinical and toxicological studies, as well as establishing potential associations between tea consumption and disease prevention.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140990762","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
N. Kwon, Jaehyeong Park, Seon Yeong Kim, B. Ko, J. Cheong, Jin Young Kim
Continuous Li monitoring is vital in ensuring the safety and treatment efficacy of probationers with psychotic disorders, such as bipolar disorder, depression, and mania. This study introduced a validated quantitative analysis method using ion chromatography (IC) to monitor Li+ concentration in urine. The methodology involved centrifuging the urine sample, diluting the supernatant with deionized water, and subsequent IC analysis using guard and analytical columns for precise Li+ concentration measurement. The method quantified Li+ within the range of 2–400 ng/mL, demonstrating its excellent linearity (r2 = 0.9983) with a weighting factor of 1/x. Precision levels below 12.8% were observed for both intraday and interday measurements with an accuracy of −5.9% to 15.2%. The detection limit was identified as 0.12 ng/mL. The method conformed to analytical standards in terms of selectivity, matrix effect, process efficiency, dilution integrity, and stability. Moreover, the method distinctly quantified Li+ while effectively eliminating interference from Na+, which had a similar retention time as Li+ with higher concentrations. Further, the developed method was successfully applied to analyze forensic urine samples of Li users, demonstrating its applicability for medication compliance monitoring using urine samples of mentally disordered probationers.
{"title":"Ion chromatography‐based determination of lithium in human urine for monitoring medication compliance","authors":"N. Kwon, Jaehyeong Park, Seon Yeong Kim, B. Ko, J. Cheong, Jin Young Kim","doi":"10.1002/sscp.202400057","DOIUrl":"https://doi.org/10.1002/sscp.202400057","url":null,"abstract":"Continuous Li monitoring is vital in ensuring the safety and treatment efficacy of probationers with psychotic disorders, such as bipolar disorder, depression, and mania. This study introduced a validated quantitative analysis method using ion chromatography (IC) to monitor Li+ concentration in urine. The methodology involved centrifuging the urine sample, diluting the supernatant with deionized water, and subsequent IC analysis using guard and analytical columns for precise Li+ concentration measurement. The method quantified Li+ within the range of 2–400 ng/mL, demonstrating its excellent linearity (r2 = 0.9983) with a weighting factor of 1/x. Precision levels below 12.8% were observed for both intraday and interday measurements with an accuracy of −5.9% to 15.2%. The detection limit was identified as 0.12 ng/mL. The method conformed to analytical standards in terms of selectivity, matrix effect, process efficiency, dilution integrity, and stability. Moreover, the method distinctly quantified Li+ while effectively eliminating interference from Na+, which had a similar retention time as Li+ with higher concentrations. Further, the developed method was successfully applied to analyze forensic urine samples of Li users, demonstrating its applicability for medication compliance monitoring using urine samples of mentally disordered probationers.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140991791","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yan Wu, Li Ma, Zengheng Xiong, Danyu Huang, Mingshan Zhang, Xinrui Yang, Long Cheng, Shuhai He, Huan Lin
Neonicotinoids (NEOs), highly selective toward insect nicotinic acetylcholine receptors, are extensively used due to their effectiveness against pests and relative non‐toxicity to vertebrates. However, their prolonged persistence in soil and water has led to frequent detection in food and environmental samples, posing significant environmental and health concerns. Recent research indicates these pesticides infiltrate aquatic ecosystems, threatening aquatic life and human health. Here, we improved the ultra‐performance liquid chromatography‐mass spectrometry method for detecting NEOs in water samples, increasing its sensitivity to fulfill forthcoming detection needs. This approach enables the simultaneous quantification of eight NEOs and five NEO metabolites in diverse water sources, including tap, surface, groundwater, sewage, and seawater. Our method achieves remarkably low detection limits for direct injection (0.78–1.7 ng/L) and solid‐phase extraction methods (0.13–0.25 ng/L). Critically, our findings reveal that boiling domestic drinking water doesn't degrade NEOs; instead, it increases their concentration due to water evaporation. A 6‐min boiling period can amplify pesticide concentration by 4–5 times, presenting a significant hazard in culinary practices of specific regions where prolonged cooking could lead to alarmingly high levels of these insecticides. This research underscores the importance of monitoring and mitigating NEO contamination in water sources to safeguard environmental and public health.
{"title":"Simultaneous determination of eight neonicotinoid insecticides and five metabolites in water samples by liquid chromatography‐tandem mass spectrometry unveils an overlooked risk","authors":"Yan Wu, Li Ma, Zengheng Xiong, Danyu Huang, Mingshan Zhang, Xinrui Yang, Long Cheng, Shuhai He, Huan Lin","doi":"10.1002/sscp.202400009","DOIUrl":"https://doi.org/10.1002/sscp.202400009","url":null,"abstract":"Neonicotinoids (NEOs), highly selective toward insect nicotinic acetylcholine receptors, are extensively used due to their effectiveness against pests and relative non‐toxicity to vertebrates. However, their prolonged persistence in soil and water has led to frequent detection in food and environmental samples, posing significant environmental and health concerns. Recent research indicates these pesticides infiltrate aquatic ecosystems, threatening aquatic life and human health. Here, we improved the ultra‐performance liquid chromatography‐mass spectrometry method for detecting NEOs in water samples, increasing its sensitivity to fulfill forthcoming detection needs. This approach enables the simultaneous quantification of eight NEOs and five NEO metabolites in diverse water sources, including tap, surface, groundwater, sewage, and seawater. Our method achieves remarkably low detection limits for direct injection (0.78–1.7 ng/L) and solid‐phase extraction methods (0.13–0.25 ng/L). Critically, our findings reveal that boiling domestic drinking water doesn't degrade NEOs; instead, it increases their concentration due to water evaporation. A 6‐min boiling period can amplify pesticide concentration by 4–5 times, presenting a significant hazard in culinary practices of specific regions where prolonged cooking could lead to alarmingly high levels of these insecticides. This research underscores the importance of monitoring and mitigating NEO contamination in water sources to safeguard environmental and public health.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140992065","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Cyproheptadine hydrochloride (CYP) is a typical antihistamine with antiserotonergic, blocking H1 receptor, anticholine, anti‐inflammatory and anti‐allergic effects. To investigate the pharmacokinetics, biodistribution, and excretion, the liquid chromatography‐tandem mass spectrometry (LC‐MS/MS) method was established and validated the CYP concentrations in the plasma of beagle dogs and the biological matrix of mice. CYP was quickly absorbed into the bloodstream and widely distributed to various tissues. The area under the curve (AUC)0–t and peak concentration of CYP were increased with the dose after administration. At the equal dose, the bioavailability of intramuscular injection in mice and beagle dogs was 81.1% and 79.1%. The tissue distribution experiments suggested that CYP would not accumulate for a long time in vivo. CYP levels in tissues peaked after 15 min of injection, and the drug concentrations in the kidney and lung were higher than those in other tissues. For excretion, the cumulative urinary excretion of CYP within 156 h after intramuscular injection in mice accounted for (1.2 ± 0.1)% of the total administration dose. The feces excretion of the drug prototype was below the lower limit of quantitation. High sensitivity and strong specificity are observed based on the established method of LC‐MS/MS, which was successfully applied to the pharmacokinetics, tissue distribution, and excretion studies of CYP.
{"title":"Pharmacokinetics of cyproheptadine hydrochloride in mice and beagle dogs, tissue distribution, and excretion properties of cyproheptadine hydrochloride in mice","authors":"Ting Liu, Chunying Cui, Jielin Zhou","doi":"10.1002/sscp.202400066","DOIUrl":"https://doi.org/10.1002/sscp.202400066","url":null,"abstract":"Cyproheptadine hydrochloride (CYP) is a typical antihistamine with antiserotonergic, blocking H1 receptor, anticholine, anti‐inflammatory and anti‐allergic effects. To investigate the pharmacokinetics, biodistribution, and excretion, the liquid chromatography‐tandem mass spectrometry (LC‐MS/MS) method was established and validated the CYP concentrations in the plasma of beagle dogs and the biological matrix of mice. CYP was quickly absorbed into the bloodstream and widely distributed to various tissues. The area under the curve (AUC)0–t and peak concentration of CYP were increased with the dose after administration. At the equal dose, the bioavailability of intramuscular injection in mice and beagle dogs was 81.1% and 79.1%. The tissue distribution experiments suggested that CYP would not accumulate for a long time in vivo. CYP levels in tissues peaked after 15 min of injection, and the drug concentrations in the kidney and lung were higher than those in other tissues. For excretion, the cumulative urinary excretion of CYP within 156 h after intramuscular injection in mice accounted for (1.2 ± 0.1)% of the total administration dose. The feces excretion of the drug prototype was below the lower limit of quantitation. High sensitivity and strong specificity are observed based on the established method of LC‐MS/MS, which was successfully applied to the pharmacokinetics, tissue distribution, and excretion studies of CYP.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2024-05-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140993134","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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