{"title":"用激光诱导荧光毛细管电泳分析金和金接枝的磁性纳米颗粒预富集后呼出液中的生物硫醇","authors":"Jiří Volánek , Petr Kubáň","doi":"10.1016/j.talanta.2025.128550","DOIUrl":null,"url":null,"abstract":"<div><div>Gold and Fe<sub>3</sub>O<sub>4</sub>–Au composite magnetic nanoparticles were employed for the selective extraction and preconcentration of cysteine, homocysteine, and glutathione from exhaled breath condensate (EBC) samples. Using a cascade type EBC sampler, 1 mL of EBC was collected, and biological thiols were extracted and preconcentrated with preconcentration factors ranging from 8 to 34. The extraction process involved binding thiols to nanoparticles, separating them from the sample matrix, and then releasing them from the nanoparticles using dithiothreitol (DTT). The preconcentrated thiols were subsequently derivatized with naphthalene-2,3-dicarboxaldehyde. This derivatization method allowed for the use of high DTT concentrations without interfering with the separation step due to the presence of the –SH group. The separation was performed in a 10 mM sodium borate buffer at pH 10. A cost-effective 405 nm laser-induced fluorescence detector was constructed and utilized for detection. The method was linear between 0 and 50 nM, with R<sup>2</sup> in the range of 0.9948–0.9998 and LODs of 0.24 nM, 0.63 nM and 0.71 nM were achieved for cysteine, homocysteine and glutathione, respectively. The precision expressed as RSD of peak areas was between 6.8 and 8.7 %. The average relative spike recoveries for cysteine, homocysteine and glutathione in EBC samples were 76 %, 84 %, and 80 %, respectively, with a range of 54 %–112 % across three different concentration levels. Additionally, Fe<sub>3</sub>O<sub>4</sub>–Au magnetic nanoparticles were tested and enabled rapid magnetic separation, reducing processing time and highlighting the potential for automation. This optimized preconcentration procedure demonstrated efficient biothiol extraction with very low detection limits, enabling, for the first time, the simultaneous analysis of these three thiols in EBC.</div></div>","PeriodicalId":435,"journal":{"name":"Talanta","volume":"297 ","pages":"Article 128550"},"PeriodicalIF":6.1000,"publicationDate":"2025-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Capillary electrophoresis with laser induced fluorescence for the analysis of biological thiols in exhaled breath condensate after preconcentration using gold and gold-grafted magnetic nanoparticles\",\"authors\":\"Jiří Volánek , Petr Kubáň\",\"doi\":\"10.1016/j.talanta.2025.128550\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>Gold and Fe<sub>3</sub>O<sub>4</sub>–Au composite magnetic nanoparticles were employed for the selective extraction and preconcentration of cysteine, homocysteine, and glutathione from exhaled breath condensate (EBC) samples. Using a cascade type EBC sampler, 1 mL of EBC was collected, and biological thiols were extracted and preconcentrated with preconcentration factors ranging from 8 to 34. The extraction process involved binding thiols to nanoparticles, separating them from the sample matrix, and then releasing them from the nanoparticles using dithiothreitol (DTT). The preconcentrated thiols were subsequently derivatized with naphthalene-2,3-dicarboxaldehyde. This derivatization method allowed for the use of high DTT concentrations without interfering with the separation step due to the presence of the –SH group. The separation was performed in a 10 mM sodium borate buffer at pH 10. A cost-effective 405 nm laser-induced fluorescence detector was constructed and utilized for detection. The method was linear between 0 and 50 nM, with R<sup>2</sup> in the range of 0.9948–0.9998 and LODs of 0.24 nM, 0.63 nM and 0.71 nM were achieved for cysteine, homocysteine and glutathione, respectively. The precision expressed as RSD of peak areas was between 6.8 and 8.7 %. The average relative spike recoveries for cysteine, homocysteine and glutathione in EBC samples were 76 %, 84 %, and 80 %, respectively, with a range of 54 %–112 % across three different concentration levels. Additionally, Fe<sub>3</sub>O<sub>4</sub>–Au magnetic nanoparticles were tested and enabled rapid magnetic separation, reducing processing time and highlighting the potential for automation. This optimized preconcentration procedure demonstrated efficient biothiol extraction with very low detection limits, enabling, for the first time, the simultaneous analysis of these three thiols in EBC.</div></div>\",\"PeriodicalId\":435,\"journal\":{\"name\":\"Talanta\",\"volume\":\"297 \",\"pages\":\"Article 128550\"},\"PeriodicalIF\":6.1000,\"publicationDate\":\"2025-07-04\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Talanta\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0039914025010409\",\"RegionNum\":1,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Talanta","FirstCategoryId":"92","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0039914025010409","RegionNum":1,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
Capillary electrophoresis with laser induced fluorescence for the analysis of biological thiols in exhaled breath condensate after preconcentration using gold and gold-grafted magnetic nanoparticles
Gold and Fe3O4–Au composite magnetic nanoparticles were employed for the selective extraction and preconcentration of cysteine, homocysteine, and glutathione from exhaled breath condensate (EBC) samples. Using a cascade type EBC sampler, 1 mL of EBC was collected, and biological thiols were extracted and preconcentrated with preconcentration factors ranging from 8 to 34. The extraction process involved binding thiols to nanoparticles, separating them from the sample matrix, and then releasing them from the nanoparticles using dithiothreitol (DTT). The preconcentrated thiols were subsequently derivatized with naphthalene-2,3-dicarboxaldehyde. This derivatization method allowed for the use of high DTT concentrations without interfering with the separation step due to the presence of the –SH group. The separation was performed in a 10 mM sodium borate buffer at pH 10. A cost-effective 405 nm laser-induced fluorescence detector was constructed and utilized for detection. The method was linear between 0 and 50 nM, with R2 in the range of 0.9948–0.9998 and LODs of 0.24 nM, 0.63 nM and 0.71 nM were achieved for cysteine, homocysteine and glutathione, respectively. The precision expressed as RSD of peak areas was between 6.8 and 8.7 %. The average relative spike recoveries for cysteine, homocysteine and glutathione in EBC samples were 76 %, 84 %, and 80 %, respectively, with a range of 54 %–112 % across three different concentration levels. Additionally, Fe3O4–Au magnetic nanoparticles were tested and enabled rapid magnetic separation, reducing processing time and highlighting the potential for automation. This optimized preconcentration procedure demonstrated efficient biothiol extraction with very low detection limits, enabling, for the first time, the simultaneous analysis of these three thiols in EBC.
期刊介绍:
Talanta provides a forum for the publication of original research papers, short communications, and critical reviews in all branches of pure and applied analytical chemistry. Papers are evaluated based on established guidelines, including the fundamental nature of the study, scientific novelty, substantial improvement or advantage over existing technology or methods, and demonstrated analytical applicability. Original research papers on fundamental studies, and on novel sensor and instrumentation developments, are encouraged. Novel or improved applications in areas such as clinical and biological chemistry, environmental analysis, geochemistry, materials science and engineering, and analytical platforms for omics development are welcome.
Analytical performance of methods should be determined, including interference and matrix effects, and methods should be validated by comparison with a standard method, or analysis of a certified reference material. Simple spiking recoveries may not be sufficient. The developed method should especially comprise information on selectivity, sensitivity, detection limits, accuracy, and reliability. However, applying official validation or robustness studies to a routine method or technique does not necessarily constitute novelty. Proper statistical treatment of the data should be provided. Relevant literature should be cited, including related publications by the authors, and authors should discuss how their proposed methodology compares with previously reported methods.