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Electrospray ionization mass spectrometry from discrete nanoliter-sized sample volumes
KTH, School of Chemical Science and Engineering (CHE), Chemistry, Analytical Chemistry (closed 20110630).
KTH, School of Chemical Science and Engineering (CHE), Chemistry, Analytical Chemistry (closed 20110630).
KTH, School of Chemical Science and Engineering (CHE), Chemistry, Analytical Chemistry (closed 20110630).ORCID iD: 0000-0002-3444-9987
KTH, School of Chemical Science and Engineering (CHE), Chemistry, Analytical Chemistry (closed 20110630).
2010 (English)In: Rapid Communications in Mass Spectrometry, ISSN 0951-4198, E-ISSN 1097-0231, Vol. 24, no 17, 2561-2568 p.Article in journal (Refereed) Published
Abstract [en]

We describe a method for nanoelectrospray ionization mass spectrometry (nESI-MS) of very small sample volumes. Nanoliter-sized sample droplets were taken up by suction into a nanoelectrospray needle from a silicon microchip prior to ESI. To avoid a rapid evaporation of the small sample volumes, all manipulation steps were performed under a cover of fluorocarbon liquid. Sample volumes down to 1.5 nL were successfully analyzed, and an absolute limit of detection of 105 attomole of insulin (chain B, oxidized) was obtained. The open access to the sample droplets on the silicon chip provides the possibility to add reagents to the sample droplets and perform chemical reactions under an extended period of time. This was demonstrated in an example where we performed a tryptic digestion of cytochrome C in a nanoliter-sized sample volume for 2.5h, followed by monitoring the outcome of the reaction with nESI-MS. The technology was also utilized for tandem mass spectrometry (MS/MS) sequencing analysis of a 2 nL solution of angiotensin I.

Place, publisher, year, edition, pages
2010. Vol. 24, no 17, 2561-2568 p.
National Category
Analytical Chemistry
Identifiers
URN: urn:nbn:se:kth:diva-26071DOI: 10.1002/rcm.4674ISI: 000281355000011Scopus ID: 2-s2.0-77955386519OAI: oai:DiVA.org:kth-26071DiVA: diva2:369682
Note

QC 20101111

Available from: 2010-11-11 Created: 2010-11-11 Last updated: 2017-06-08Bibliographically 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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