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Updated: Jun 10, 2025

Sheathless Capillary Electrophoresis–Mass Spectrometry for Metabolic Profiling of Biological Samples
Published on: October 1, 2016
A robust polymetallic-coated sheathless interface with high acid and alkali resistance for coupling capillary
Xiaozhong Hu1, Wenqing Gao1, Rong Liu1
1Institute of Mass Spectrometry, Zhejiang Engineering Research Center of Advanced Mass Spectrometry and Clinical Application, School of Material Science and Chemical Engineering, Ningbo University, Ningbo, 315211, PR China; Zhenhai Institute of Mass Spectrometry, Ningbo, 315211, PR China; School of Material Science and Chemical Engineering, Ningbo University, Ningbo, 315211, PR China.
Abstract:
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.
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