Chromatographia

, Volume 76, Issue 17–18, pp 1079–1086 | Cite as

A Fast and Effective Method for Packing Nano-LC Columns with Solid-Core Nano Particles Based on the Synergic Effect of Temperature, Slurry Composition, Sonication and Pressure

  • Fabiana Capriotti
  • Irene Leonardis
  • Achille Cappiello
  • Giorgio Famiglini
  • Pierangela Palma
Original
First Online:
Received:
Revised:
Accepted:

Abstract

Nano-LC columns of different lengths (14–35 cm), 75 μm i.d., were packed with solid-core C18 particles using a conventional HPLC system at low pressure (375 bar) and without expensive tools and fittings. Solid-core particles consist of a solid, non-porous core surrounded with a shell of a porous layer with a very narrow particle size distribution. This geometry allows a faster diffusion of the analytes compared to porous particles, reducing the C term of the Knox plot. Different slurries of packing material were evaluated and tested. The packing procedure was carried out at room temperature and at 70 °C to evaluate the influence of this parameter on the overall process. The synergic action of pressure, temperature and sonication contributed to columns of various lengths in the packing process. The columns were tested at room temperature taking into account the following parameters: Knox plots, specific permeability and peak capacity. Reduced heights of theoretical plates, h, ranged between 3.8 and 5.1 at ν between 2 and 6. An LC-MS test was carried out with a Direct-EI LC-MS instrument.

Keywords

Nano-LC columns Solid-core particles stationary phase LC-MS analysis 
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References

  1. 1.
    Horváth C, Preiss BA, Lipsky SR (1967) Anal Chem 39:1422–1428CrossRefGoogle Scholar
  2. 2.
    Horvath C, Lipsky SR (1969) J Chromatogr Sci 7:109–116CrossRefGoogle Scholar
  3. 3.
    Kirkland JJ (1969) J Chromatogr Sci 7:7–12CrossRefGoogle Scholar
  4. 4.
    Kirkland JJ (1969) US Patent 3:505–785Google Scholar
  5. 5.
    Kirkland JJ (1969) Anal Chem 41:218–220CrossRefGoogle Scholar
  6. 6.
    Guoichon G, Gritti F (2011) J Chromatogr A 1218:1915–1938CrossRefGoogle Scholar
  7. 7.
    De Stefano JJ, Langlois TJ, Kirkland JJ (2008) J Chromatogr Sci 46:254–260CrossRefGoogle Scholar
  8. 8.
    Cavazzini A, Gritti F, Kaczmarski K, Marchetti N, Guiochon G (2007) Anal Chem 79:5972–5979CrossRefGoogle Scholar
  9. 9.
    Gritti F, Guiochon G, Cavazzini A, Marchetti N (2007) J Chromatogr A 1157:289–303CrossRefGoogle Scholar
  10. 10.
    Gritti F, Leonardis I, Shock D, Stevenson P, Shalliker A, Guiochon G (2010) J Chromatogr A 1217:1589–1603CrossRefGoogle Scholar
  11. 11.
    Fekete S, Olah E, Fekete J (2011) J Chromatogr A 1228:57–71Google Scholar
  12. 12.
    Baker J, Vinci JC, Moore AD, Colón LA (2010) J Sep Sci 33:2547–2557CrossRefGoogle Scholar
  13. 13.
    Gritti F, Guiochon G (2012) J Chromatogr A 1228:2–19CrossRefGoogle Scholar
  14. 14.
    Fekete S, Fekete J (2011) Talanta 84:416–423CrossRefGoogle Scholar
  15. 15.
    Kirkland JJ (1992) Anal Chem 64:1239–1245CrossRefGoogle Scholar
  16. 16.
    Felinger A (2011) J Chromatogr A 1218:1939–1941CrossRefGoogle Scholar
  17. 17.
    Causon TJ, Broeckhoven K, Hilder EF, Shellie RA, Desmet G, Eeltink S (2011) J Sep Sci 34:877–887CrossRefGoogle Scholar
  18. 18.
    Knox JH (1999) J Chromatogr A 831:3–15CrossRefGoogle Scholar
  19. 19.
    Lanças FM, Rodrigues JC, de Freitas SS (2004) J Sep Sci 27:1475–1482CrossRefGoogle Scholar
  20. 20.
    Unger KK, Skudas R, Schulte MM (2008) J Chromatogr A 1184:393–415CrossRefGoogle Scholar
  21. 21.
    Kirkland JJ (1971) J Chromatogr Sci 9:206–214CrossRefGoogle Scholar
  22. 22.
    Asshauer J, Halasz I (1974) J Chromatogr Sci 12:139–147CrossRefGoogle Scholar
  23. 23.
    Verzele M (1984) J Chromatogr A 295:81–87CrossRefGoogle Scholar
  24. 24.
    Liao JC, Ponzo JL (1982) J Chromatogr Sci 20:14–18CrossRefGoogle Scholar
  25. 25.
    Karlsson K, Novotny M (1988) Anal Chem 60:1662–1665CrossRefGoogle Scholar
  26. 26.
    Ehlert S, Roesler T, Tallarek U (2008) J Sep Sci 31:1719–1728CrossRefGoogle Scholar
  27. 27.
    Fermier AM, Colón LA (1998) J Microcolumn Sep 10:439–447CrossRefGoogle Scholar
  28. 28.
    Bruns S, Tallarek U (2011) J Chromatogr A 1218:1849–1860CrossRefGoogle Scholar
  29. 29.
    Daneyko A, Hlushkou D, Khirevich S, Tallarek U (2012) J Chromatogr A 1257:98–115CrossRefGoogle Scholar
  30. 30.
    Shih CY, Chen Y, Xie J, He Q, Tai YC (2006) J Chromatogr A 1111:272–278CrossRefGoogle Scholar
  31. 31.
    Patel KD, Jerkovich AD, Link JC, Jorgenson JW (2004) Anal Chem 76:5777–5786CrossRefGoogle Scholar
  32. 32.
    Fanali S, Aturki Z, D’Orazio G, Rocco A (2007) J Chromatogr A 1150:252–258CrossRefGoogle Scholar
  33. 33.
    D’Orazio G, Rocchi S, Fanali S (2012) J Chromatogr A 1255:277–285CrossRefGoogle Scholar
  34. 34.
    Cappiello A, Famiglini G, Pierini E, Palma P, Trufelli H (2007) Anal Chem 79:5364–5372CrossRefGoogle Scholar
  35. 35.
    Cappiello A, Famiglini G, Palma P, Siviero A (2005) Mass Spectrom Rev 24:978–989CrossRefGoogle Scholar
  36. 36.
    Cappiello A, Palma P (2007) In: Cappiello A (ed) Advances in LC-MS instrumentation, vol 72 (Journal of Chromatography Library), Elsevier, AmsterdamGoogle Scholar
  37. 37.
    Cappiello A, Famiglini G, Palma P, Siviero A (2005) Mass Spectrom Rev 24:978–989CrossRefGoogle Scholar
  38. 38.
    Knox H, Ross P (1997) Adv Chromatogr 37:73–119Google Scholar
  39. 39.
    Ross P LCGC Europe (2000) 13:310–319Google Scholar
  40. 40.
    Pereira L, Aspey S, Ritchie H (2007) J Sep Sci 30:1115–1124CrossRefGoogle Scholar
  41. 41.
    Carr PW, Hu Y, Li J (1997) Anal Chem 69:3884–3888CrossRefGoogle Scholar
  42. 42.
    Sun J, Carr PW (1995) Anal Chem 67:3717–3721CrossRefGoogle Scholar
  43. 43.
    Leonardis I, Capriotti F, Cappiello A, Famiglini G, Palma P (2012) J Sep Sci 35:1589–1595CrossRefGoogle Scholar
  44. 44.
    Bristow PA, Knox JH (1977) Chromatographia 10:279–289CrossRefGoogle Scholar
  45. 45.
    Mayors RE (2004) LCGC Asia Pacific 7:1124–1133Google Scholar
  46. 46.
    Snyder LR, Kirkland JJ, Dolan JW (2010) Introduction to modern liquid chromatography, 3rd edn. Wiley, New YorkGoogle Scholar
  47. 47.
    Neue UD (1997) HPLC Columns: theory technology and practice. Wiley-VCH, New YorkGoogle Scholar
  48. 48.
    Baker JS, Vinci JC, Moore AD, Colón LA (2010) J Sep Sci 33:2547–2557CrossRefGoogle Scholar
  49. 49.
    Fanali S, Camera E, Chankevetadze B, D’Orazio G, Quaglia MG (2004) J Pharm Biomed Anal 35:331–337CrossRefGoogle Scholar

Copyright information

© Springer-Verlag Berlin Heidelberg 2013

Authors and Affiliations

  • Fabiana Capriotti
    • 1
  • Irene Leonardis
    • 1
  • Achille Cappiello
    • 1
  • Giorgio Famiglini
    • 1
  • Pierangela Palma
    • 1
  1. 1.Università di Urbino “Carlo Bo”, DiSTeVA, Laboratorio LC-MSUrbinoItaly

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