Abstract
Surface-assisted, laser desorption ionization (SALDI) time-of-flight mass spectra of proteins and peptides have been obtained from bulk frozen aqueous solutions by adding solid organic powders to the solutions before freezing. Abundant analyte ions were obtained with a 3.28 µm Nd:YAG/OPO laser. 20 compounds were evaluated as solid additives, and 16 yielded protein mass spectra. Successful solids included compounds like pyrene, aspartic acid, and polystyrene. The best results were obtained with nicotinic acid and indole-2-carboxylic acid, which yielded protein mass spectra anywhere on the sample and with every laser shot. Compared with ultraviolet-matrix-assisted laser desorption ionization on the same instrument, cryo-IR-SALDI had a comparable detection limit (≈1 µM), a lower mass resolution for peptides, and a higher mass resolution for large proteins. Approximately 2500 cryo-IR-SALDI mass spectra were obtained from a single spot on a 0.3-mm-thick frozen sample before the metal surface was reached. About 0.1 nL of frozen solution was desorbed per laser shot. The extent of protein charging varied between the SALDI solids used. With thymine, myoglobin charge states up to MH +1212 were observed. It is tentatively concluded that observed ions are preformed in the frozen sample.
Similar content being viewed by others
References
Hillenkamp, F.; Karas, M.; Beavis, R. C.; Chait, B. T. Anal. Chem. 1991, 63, 1193A-1203A.
Stults, J. T. Curr. Opin. Struct. Biol. 1997, 5, 691–698.
Karas, M.; Bachmann, D.; Bahr, U.; Hillenkamp, F. Int. J. Mass Spectrom. Ion. Processes 1987, 78, 53–68.
Fenn, J. B.; Mann, M.; Meng, C. K.; Wong, S. F.; Whitehouse, C. M. Science 1989, 246, 64–71.
Low Temperature Biotechnology; The American Society of Mechanical Engineers: New York, 1988.
Fahy, G. M.; Lilley, T. H.; Lindsell, H.; Douglas, M. S.; Meryman, H. T. Cryobiology 1990, 3, 1630.
Williams, P. Int. J. Mass Spectrom. Ion. Processes 1994, 131, 335–344.
Berkenkamp, S.; Karas, M.; Hillenkamp, F. Proc. Natl. Acad. Sci. USA 1996, 93, 7003–7007.
Eisenberg, D.; Kauzmann, W. The Structure and Properties of Water; Oxford: New York, 1969; 228–253.
Overberg, A.; Karas, M.; Bahr, U.; Kaufmann, R.; Hillenkamp, F. Rapid Commun. Mass Spectrom. 1990, 4, 293–296.
Overberg, A.; Karas, M.; Hillenkamp, F. Rapid Commun. Mass Spectrom. 1991, 5, 128–131.
Berkenkamp, S.; Karas, M.; Hillenkamp, F. In Proceedings of the 43rd ASMS Conference on Mass Spectrometry and Allied Topics; Atlanta, GA, May 21–26, 1995; p 1247.
Nordhoff, E.; Ingendoh, A.; Cramer, R.; Overberg, A.; Stahl, B.; Karas, M.; Hillenkamp, F.; Crain, P. F. Rapid Commun. Mass Spectrom. 1992, 6, 771–776.
Cramer, R.; Hillenkamp, F.; Haglund, R. F. J. Am. Soc. Mass. Spectrom. 1996, 7, 1187–1193.
Berkenkamp, S.; Menzel, C.; Karas, M.; Hillenkamp, F. Rapid Commun. Mass Spectrom. 1997, 11, 1399–1406.
Niu, S.; Zhang, W.; Chait, B. T. J. Am. Soc. Mass Spectrom. 1998, 9, 1–7.
Tanaka, K.; Waki, H.; Idao, Y.; Akita, S.; Yoshida, Y.; Yoshida, T. Rapid Commun. Mass Spectrom. 1988, 2, 151–153.
Siegel, M. M.; Kunz, A.; Bell, D.; Berkenkamp, S.; Karas, M.; Ingendoh, A.; Hillenkamp, F. In Proceedings of the 42nd ASMS Conference on Mass Spectrometry and Allied Topics; Chicago, IL, May 29–June 3, 1994; p 967.
Juhasz, P.; Costello, C. E. Rapid Commun. Mass Spectrom. 1993, 7, 343–351.
Juhasz, P.; Biemann, K. Proc. Natl. Acad. Sci. USA 1994, 91, 4333–4337.
Sadeghi, M.; Olumee, Z.; Tang, X.; Vertes, A.; Jiang, Z. X.; Henderson, A. J.; Lee, H. S.; Prasad, C. R. Rapid Commun. Mass Spectrom. 1997, 11, 393–397.
Cummings, J. P.; Walsh, J. T., Jr. Appl. Phys. Lett. 1993, 62, 1988–1990.
Vodopyanov, K. L. J. Chem. Phys. 1991, 94, 5389.
Cummings, J. P.; Walsh, J. T., Jr. SPIE 1992, 1646, 242–253.
Nelson, R. W.; Rainbow, M. J.; Lohr, D. E.; Williams, P. Science 1989, 246, 1585–1587.
Nelson, R. W.; Thomas, R. M.; Williams, P. Rapid Commun. Mass Spectrom. 1990, 4, 348–351.
Schieltz, D. M.; Chou, C. W.; Luo, C. W.; Thomas, R. M.; Williams, P. Rapid Commun. Mass Spectrom. 1992, 6, 631–636.
Williams, P.; Nelson, R. W. In Methods and Mechanisms for Producing Ions from Large Molecules; Standing, K. G.; Ens, W., Eds.; Plenum: New York, 1991; pp 265–273.
Hunter, J. M.; Lin, H.; Becker, C. H. Anal. Chem. 1997, 69, 3608–3612.
Alimpiev, S. S.; Belov, M. E.; Mlinsky, V. V.; Nikiforov, S. S. Analyst 1994, 119, 579–582.
Alimpiev, S. S.; Mlynski, V. V.; Belov, M. E.; Nikiforov, S. M. Anal. Chem. 1995, 67, 181–186.
Belov, M. E.; Alimpiev, S. S.; Mlynsky, V. V.; Nikiforov, S. M.; Derrick, P. J. Rapid Commun. Mass Spectrom. 1995, 9, 1431–1436.
Sunner, J.; Dratz, E.; Chen, Y. C. Anal. Chem. 1995, 67, 4335–4342.
Alimpiev, S.; Chen, Y.-C. Dratz, E.; Kraft, P.; Sunner, J. In Proceedings of the 44th ASMS Conference on Mass Spectrometry and Allied Topics; Portland, OR, May 12–16, 1996; p 641.
Touloukian, Y. S.; Powell, R. W.; Ho, C. Y.; Klemens, P. G. Thermophysical Properties of Matter. Vol. 2; Plenum: New York, 1970.
Lane, L. B. Ind. Eng. Chem. 1925, 17, 924.
Boutron, P. Cryobiology 1984, 21, 183–191.
Alimpiev, S.; Dratz, E.; Kraft, P.; Sunner, J. In Proceedings of the 44th ASMS Conference on Mass Spectrometry and Allied Topics; Portland, Oregon, May 12–16, 1996; p 644.
Sunner, J. Org. Mass Spectrom. 1993, 28, 805–823.
Dreisewerd, K.; Schurenberg, M.; Karas, M.; Hillenkamp, F. Int. J. Mass Spectrom. Ion. Processes 1995, 141, 127–148.
Bohon, R. L.; Conway, W. T. Thermochimica Acta 1972, 4, 321–341.
Franks, F. In Developments in Biological Standardization. International Symposium on Biological Freeze-Drying and Formulation, Bethesda, USA, 1990; Karger: Basel, 1991; pp 9–19.
Feng, R.; Konishi, Y. J. Am. Soc. Mass Spectrom. 1993, 4, 638–645.
Buttrill, S. E., Jr., Fleming, R. H.; Rossi, M.; Gohl, W.; Goeller, L. N. In Proceedings of the 29th Annual Conference on Mass Spectrometry and Allied Topics; Minneapolis, MN, May 24–29, 1981; pp 594–595.
Sunner, J.; Ikonomou, M. G.; Kebarle, P. Int. J. Mass Spectrom. Ion. Processes 1988, 82, 221–237.
Vestal, M. L.; Juhasz, P.; Martin, S. A. Rapid Commun. Mass Spectrom. 1995, 9, 1044–1050.
Brown, R. S.; Lennon, J. J. Anal. Chem. 1995, 67, 1998–2003.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Kraft, P., Alimpiev, S., Dratz, E. et al. Infrared, surface-assisted laser desorption ionization mass spectrometry on frozen aqueous solutions of proteins and peptides using suspensions of organic solids. J Am Soc Mass Spectrom 9, 912–924 (1998). https://doi.org/10.1016/S1044-0305(98)00063-4
Received:
Revised:
Accepted:
Issue Date:
DOI: https://doi.org/10.1016/S1044-0305(98)00063-4