{"title":"用于毛细管电泳与质谱联用的坚固耐用、耐酸碱的多金属涂层无护套接口。","authors":"Xiaozhong Hu, Wenqing Gao, Rong Liu, Chen Tang, Huanming Wu, Jiancheng Yu, Yuheng Wang, Keqi Tang","doi":"10.1016/j.talanta.2024.127045","DOIUrl":null,"url":null,"abstract":"<p><p>A robust interface for coupling capillary electrophoresis (CE) to mass spectrometry (MS) was critical to maintain high separation efficiency of CE while achieving high sensitivity of MS. Current interfaces often suffer from problems such as reproducibility and ruggedness. For this purpose, a new polymetallic-coated sheathless interface was developed for the coupling of CE with MS. The electrical contact of the interface was achieved by etching one end of the fused silica capillary into a tapered tip using hydrofluoric acid (HF) solution, and then depositing a thin layer of chromium followed by a layer of platinum on it via physical vapor deposition technique. The performance of the new sheathless interface was systematically evaluated for the effect of flow rate and electrospray ionization (ESI) voltage on MS signal intensity, as well as the sample loading volume on CE separation efficiency and repeatability by using peptide standards and tryptic digest of bovine serum albumin (BSA). The interface was capable of generating stable electrospray even at ultra-low flow rate of 12.2 nL/min. In addition, the acid and alkali resistance of the polymetallic-coated emitter was tested by immersing it into 1 M HCL and 1 M NaOH solution, respectively. The results showed that polymetallic coating was still intact even after continuous immersion in the alkaline solution for 8 days (192 h) and a longer period in the acidic solution, indicating its excellent chemical stability. All the experimental results indicated that the sheathless interface fabricated by the new method in this study was robust and stable, making it promising for both sensitive and robust CE-MS sample analysis.</p>","PeriodicalId":435,"journal":{"name":"Talanta","volume":"282 ","pages":"127045"},"PeriodicalIF":5.6000,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"A robust polymetallic-coated sheathless interface with high acid and alkali resistance for coupling capillary electrophoresis with mass spectrometry.\",\"authors\":\"Xiaozhong Hu, Wenqing Gao, Rong Liu, Chen Tang, Huanming Wu, Jiancheng Yu, Yuheng Wang, Keqi Tang\",\"doi\":\"10.1016/j.talanta.2024.127045\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><p>A robust interface for coupling capillary electrophoresis (CE) to mass spectrometry (MS) was critical to maintain high separation efficiency of CE while achieving high sensitivity of MS. 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In addition, the acid and alkali resistance of the polymetallic-coated emitter was tested by immersing it into 1 M HCL and 1 M NaOH solution, respectively. The results showed that polymetallic coating was still intact even after continuous immersion in the alkaline solution for 8 days (192 h) and a longer period in the acidic solution, indicating its excellent chemical stability. 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引用次数: 0
摘要
要保持毛细管电泳(CE)的高分离效率,同时实现质谱(MS)的高灵敏度,必须有一个强大的接口将毛细管电泳(CE)与质谱(MS)耦合起来。目前的接口往往存在可重复性和坚固性等问题。为此,我们开发了一种新型聚金属涂层无护套接口,用于 CE 与 MS 的耦合。使用氢氟酸(HF)溶液将熔融石英毛细管的一端蚀刻成锥形尖端,然后通过物理气相沉积技术在其上沉积一薄层铬和一薄层铂,从而实现接口的电接触。通过使用肽标准品和牛血清白蛋白(BSA)胰蛋白酶消化物,系统评估了流速和电喷雾离子化(ESI)电压对质谱信号强度的影响,以及样品装载量对 CE 分离效率和重复性的影响,从而确定了新型无鞘接口的性能。即使在 12.2 nL/min 的超低流速下,该界面也能产生稳定的电喷雾。此外,还将多金属涂层发射器分别浸入 1 M HCL 和 1 M NaOH 溶液中测试其耐酸碱性。结果表明,即使在碱性溶液中连续浸泡 8 天(192 小时)以及在酸性溶液中浸泡更长时间,多金属涂层仍然完好无损,这表明多金属涂层具有出色的化学稳定性。所有实验结果表明,本研究中采用新方法制作的无鞘界面坚固稳定,有望用于灵敏、稳健的 CE-MS 样品分析。
A robust polymetallic-coated sheathless interface with high acid and alkali resistance for coupling capillary electrophoresis with mass spectrometry.
A robust interface for coupling capillary electrophoresis (CE) to mass spectrometry (MS) was critical to maintain high separation efficiency of CE while achieving high sensitivity of MS. Current interfaces often suffer from problems such as reproducibility and ruggedness. For this purpose, a new polymetallic-coated sheathless interface was developed for the coupling of CE with MS. The electrical contact of the interface was achieved by etching one end of the fused silica capillary into a tapered tip using hydrofluoric acid (HF) solution, and then depositing a thin layer of chromium followed by a layer of platinum on it via physical vapor deposition technique. The performance of the new sheathless interface was systematically evaluated for the effect of flow rate and electrospray ionization (ESI) voltage on MS signal intensity, as well as the sample loading volume on CE separation efficiency and repeatability by using peptide standards and tryptic digest of bovine serum albumin (BSA). The interface was capable of generating stable electrospray even at ultra-low flow rate of 12.2 nL/min. In addition, the acid and alkali resistance of the polymetallic-coated emitter was tested by immersing it into 1 M HCL and 1 M NaOH solution, respectively. The results showed that polymetallic coating was still intact even after continuous immersion in the alkaline solution for 8 days (192 h) and a longer period in the acidic solution, indicating its excellent chemical stability. All the experimental results indicated that the sheathless interface fabricated by the new method in this study was robust and stable, making it promising for both sensitive and robust CE-MS sample analysis.
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.