Analytical and Bioanalytical Chemistry

, Volume 404, Issue 6–7, pp 1713–1721 | Cite as

Analyzing small samples with high efficiency: capillary batch injection–capillary electrophoresis–mass spectrometry

  • Marco Grundmann
  • Frank-Michael MatysikEmail author
Original Paper


We present an experimental approach to conducting fast capillary electrophoresis–mass spectrometry (CE-MS) measurements of very small samples in the nanoliter range. This is achieved by injecting sample very efficiently into a CE-MS system. Injection efficiency represents the ratio of injected sample to the amount of sample needed for carrying out the injection process (v/v). In order to increase this injection efficiency from typical values of 10–3 to 10−7, the concept of capillary batch injection is used to build an automated, small-footprint injection device for CE-MS. This device is capable of running true multi-sample measurement series, using minimal sample volumes and delivering an injection efficiency of up to 100 %. It is compatible with both aqueous and non-aqueous background electrolytes. As an additional benefit, CE-MS separations of a catecholamine model system in capillaries of 15 cm length under conditions of high electric field strength could be accomplished in 20 s with high separation efficiency. This report details design and specifications of the injection device and shows optimal parameter choices for injections with both high injection efficiency and high separation efficiency. Furthermore, a procedure is presented to coat the tip of a fused silica capillary with a silicone elastomer which acts as a seal between two capillaries.


An approach to transfer nL-samples into the separation capillary of a CE-MS system is presented. The automated and computer-controlled setup can transfer samples with up to 100 % efficiency from the point of sampling into the separation capillary, where highly efficient and fast CE-MS separations are conducted


Injection efficiency Fast capillary electrophoresis Hyphenation Mass spectrometry Small sample Fused silica capillaries High electric field strengths Catecholamines 



Background electrolyte


Capillary batch injection


Capillary electrophoresis


Electrospray ionization


Inner diameter


Mass spectrometry


Time-of-flight mass spectrometry



We would like to thank the glass, mechanical, and electronic workshops at the University of Regensburg for their assistance in implementing the experimental setup. Financial support by the Deutsche Forschungsgemeinschaft (MA 1401/7-1) is gratefully acknowledged. This research was supported by the Research Executive Agency (REA) of the European Union under Grant Agreement number PITN-GA-2010-264772 (ITN CHEBANA).

Supplementary material

216_2012_6282_MOESM1_ESM.pdf (4 kb)
ESM 1 (PDF 4 kb)

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  1. 1.
    Kubáň P, Hauser PC (2011) Electrophoresis 32:30–42, CrossRefGoogle Scholar
  2. 2.
    Pantůčková P, Gebauer P, Boček P, Křivánková L (2011) Electrophoresis 32:43–51, CrossRefGoogle Scholar
  3. 3.
    Ramautar R, Mayboroda OA, Somsen GW, de Jong GJ (2011) Electrophoresis 32:52–65, CrossRefGoogle Scholar
  4. 4.
    Haselberg R, de Jong GJ, Somsen GW (2011) Electrophoresis 32:66–82, CrossRefGoogle Scholar
  5. 5.
    Lazar IM, Lee ED, Rockwood AL, Lee ML (1998) J Chromatogr A 829:279–288, CrossRefGoogle Scholar
  6. 6.
    Hjerten S, Valtcheva L, Elenbring K, Liao JL (1995) Electrophoresis 16:584 – 594, CrossRefGoogle Scholar
  7. 7.
    Zhong M, Lunte S (1996) Anal Chem 68:2488 – 2493, CrossRefGoogle Scholar
  8. 8.
    Müller O, Minarik M, Foret F (1998) Electrophoresis 19:1436 – 1444, CrossRefGoogle Scholar
  9. 9.
    Matysik FM (2010) Anal Bioanal Chem 397:961–965, CrossRefGoogle Scholar
  10. 10.
    Jankowski JA, Tracht S, Sweedler JV (1995) Trends Anal Chem 14:170–176, Google Scholar
  11. 11.
    Blasco S, Kortz L, Matysik FM (2009) Electrophoresis 30:1–6, CrossRefGoogle Scholar
  12. 12.
    Grundmann M, Matysik FM (2011) Anal Bioanal Chem 400:269–278, CrossRefGoogle Scholar
  13. 13.
    Grundmann M, Rothenhöfer M, Bernhardt G, Buschauer A, Matysik FM (2011) Anal Bioanal Chem 402:2617–2623, CrossRefGoogle Scholar
  14. 14.
    Kennedy RT, Watson CJ, Haskins WE, Powell DH, Strecker RE (2002) Curr Opin Chem Biol 6:659–665, CrossRefGoogle Scholar
  15. 15.
    Perry M, Li Q, Kennedy RT (2009) Anal Chim Acta 653:1–22, CrossRefGoogle Scholar
  16. 16.
    Hogan BL, Lunte SM, Stobaugh JF, Lunte CE (1994) Anal Chem 66:596–602, CrossRefGoogle Scholar
  17. 17.
  18. 18.
    Lapainis T, Sweedler JV (2008) J Chromatogr A 1184:144–158, CrossRefGoogle Scholar
  19. 19.
    Kubáň P, Engström A, Olsson JC, Thorsén G, Tryzell R, Karlberg B (1997) Anal Chim Acta 337:117–124, CrossRefGoogle Scholar
  20. 20.
    Tůma P, Opekar F, Jelínek I (2000) J Chromatogr A 883:223–230, CrossRefGoogle Scholar
  21. 21.
    Fang ZL, Liu ZS, Shen Q (1997) Anal Chim Acta 346:135–143, CrossRefGoogle Scholar
  22. 22.
    Fang ZL, Fang Q (2001) Fresenius J Anal Chem 370:978–983, CrossRefGoogle Scholar
  23. 23.
    Fu CG, Fang ZL (2000) Anal Chim Acta 422:71–79, CrossRefGoogle Scholar
  24. 24.
    Cao XD, Fang Q, Fang ZL (2004) Anal Chim Acta 513:473–479, CrossRefGoogle Scholar
  25. 25.
    Opekar F, Coufal P, Štulík K (2009) Chem Rev 109:4487 – 4499, CrossRefGoogle Scholar
  26. 26.
    Matysik FM (2006) Electrochem Commun 8:1011–1015, CrossRefGoogle Scholar

Copyright information

© Springer-Verlag 2012

Authors and Affiliations

  1. 1.Institute for Analytical Chemistry, Chemo- and BiosensorsUniversity of RegensburgRegensburgGermany

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