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New Method for Fabrication of Fused Silica Emitters with Submicrometer Orifices for Nanoelectrospray Mass Spectrometry
KTH, School of Chemical Science and Engineering (CHE), Chemistry, Analytical Chemistry.
KTH, School of Chemical Science and Engineering (CHE), Chemistry, Analytical Chemistry.
2011 (English)In: Analytical Chemistry, ISSN 0003-2700, E-ISSN 1520-6882, Vol. 83, no 20, 7771-7777 p.Article in journal (Refereed) Published
Abstract [en]

In this paper, we describe a new method for fabrication of nanoelectrospray emitters. The needles were pulled from fused silica capillary tubing, which was melted by means of a plasma, formed by electrical discharges between two pointed platinum electrodes. A key feature of the pulling device is a rotating configuration of the electrodes, which results in an even radial heating of the capillary. The construction of the setup is straightforward, and needles with a variety of shapes can be fabricated, including orifices of submicrometer dimensions. Pulled needles with long tapered tips and an orifice of 0.5 mu m were utilized for electrospray ionization mass spectrometry (ESI-MS) of discrete sample volumes down to 275 pL. The picoliter-sized samples were transferred into the tip of the needle from a silicon microchip by aspiration. To avoid a rapid evaporation of the sample, all manipulations were performed under a cover of a fluorocarbon liquid. The limit of detection was measured to be ca. 20 attomole for insulin (chain B, oxidized).

Place, publisher, year, edition, pages
2011. Vol. 83, no 20, 7771-7777 p.
Keyword [en]
ELECTROSPRAY-IONIZATION SOURCE, DISCOVERY, NANOSPRAY
National Category
Analytical Chemistry
Identifiers
URN: urn:nbn:se:kth:diva-26072DOI: 10.1021/ac201308nISI: 000295817500028Scopus ID: 2-s2.0-80054701334OAI: oai:DiVA.org:kth-26072DiVA: diva2:369689
Note
QC 20101111 Updated from manuscript to article in journal.Available from: 2010-11-11 Created: 2010-11-11 Last updated: 2017-12-12Bibliographically approved
In thesis
1. New methods for sensitive analysis with nanoelectrospray ionization mass spectrometry
Open this publication in new window or tab >>New methods for sensitive analysis with nanoelectrospray ionization mass spectrometry
2010 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

In this thesis, new methods that address some current limitations in nanoelectrospray mass spectrometry (nESI-MS) analysis are presented. One of the major objectives is the potential gain in sensitivity that can be obtained when employing the proposed techniques.

In the first part of this thesis, a new emitter, based on the generation of electrospray from a spray orifice with variable size, is presented. Electrospray is generated from an open gap between the edges of two individually mounted, pointed tips. The fabrication and evaluation of two different types of such emitters is presented; an ESI emitter fabricated from polyethylene terephtalate (Paper I), and a high-precision silicon device (Paper II). Both emitters were surface-treated in a selective way for an improved wetting of the gap and to confine the sample solution into the gap.

In the second part of this thesis, different methods for improved sensitivity of nESI-MS analysis have been developed. In Paper III, a method for nESI-MS analysis from discrete sample volumes down to 1.5 nL is presented, using commercially available nESI needles. When analyzing attomole amounts of analyte in such a small volume of sample, an increased sensitivity was obtained, compared to when analyzing equal amounts in conventional nESI-MS analysis. To be able to analyze smaller sample volumes, needles with a narrower orifice and a higher flow resistance were needed. This triggered the development of a new method for fabrication of fused silica nESI needles (Paper IV). The fabrication is based on melting of a fused silica capillary by means of a rotating plasma, prior to pulling the capillary into a fine tip. Using the described technique, needles with sub-micrometer orifices could be fabricated. Such needles enabled the analysis of sample volumes down to 275 pL, and a further improvement of the sensitivity was obtained. In a final project (Paper V), nESI-MS was used to study the aggregation behavior of Aβ peptides, related to Alzheimer’s disease. An immunoprecipitation followed by nESI-MS was employed. This technique was also utilized to study the selectivity of the antibodies utilized.

Place, publisher, year, edition, pages
Stockholm: KTH, 2010. vii, 70 p.
Series
Trita-CHE-Report, ISSN 1654-1081 ; 2010:41
Keyword
mass spectrometry, electrospray ionization, nanoelectrospray ionization, adjustable gap, emitter, miniaturization, improved sensitivity, nanoliter/picoliter sample volumes, Alzheimer’s disease, amyloid-beta (Aβ)
National Category
Analytical Chemistry
Identifiers
urn:nbn:se:kth:diva-25917 (URN)978-91-7415-751-2 (ISBN)
Public defence
2010-11-26, K1, Teknikringen 56, Stockholm, 10:00 (English)
Opponent
Supervisors
Note
QC 20101112Available from: 2010-11-12 Created: 2010-11-04 Last updated: 2010-11-12Bibliographically approved

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