Abstract
A design of experiement approach is described for the optimization of the microscopic morphology of macro-mesoporous titania monoliths that were elaborated for the chromatographic enrichment of phosphorylated compounds. The monolithic titania gels were formed via an alkoxy-derived sol–gel route in association with a phase separation mechanism. The synthesis was performed at mild temperatures of gelation using starting mixtures of titanium n-propoxide, hydrochloric acid, N-methylformamide, water, and poly (ethylene oxide). The gelation temperature and the chemical compositions of N-methylformamide, water, and poly (ethylene oxide) were chosen as the most relevant experimental factors of the sol–gel process. Using the sizes of the skeletons and macropores as morphological descriptors of the dried porous monoliths, the statistical analyses simultaneously revealed the effects and interactions between the different factors. Crack-free TiO2 monolithic rods of 8 to 10 cm long with well-defined co-continuous macropores and micro-structured skeletons were obtained after selection of the sol–gel parameters and optimization of the drying and heat-treatment steps of the gels. The bimodal texture of the rods exhibited macropores of 1.5 μm and mesopores centered at 5.2 nm with a total surface area of 140 m2 g−1. The ability of the macro-mesoporous titania rods to selectively bind phosphorylated compounds was demonstrated for O-phosphoamino acids (P-Ser, P-Thr, P-Tyr).
Similar content being viewed by others
References
Kawahara M, Nakamura H, Nakajima T (1990) J Chromatogr 515:149–158
Tani K, Suzuki Y (1997) Chromatographia 46:623–627
Tani K, Miyamoto E (1999) J Liquid Chromatogr Relat Technol 22:857–871
Winkler J, Marme S (2000) J Chromatogr A 888:51–62
Kimura Y, Shibasaki S, Morisato K, Ishizuka N, Minakuchi H, Nakanishi K, Matsuo M, Amachi T, Ueda M, Ueda K (2004) Anal Biochem 326:262–266
Nawrocki J, Dunlap C, McCormick A, Carr PW (2004) J Chromatogr A 1028:1–30
Zhou T, Lucy CA (2008) J Chromatogr A 1187:87–93
Masatake O, Tani K, Masaki T, Hitoshi K, Nobutoshi K (2009) Chromatographia 70:533–537
Zhou T, Lucy CA (2010) J Chromatogr A 1217:82–88
Abi Jaoudé M, Randon J (2011) J Chromatogr A 1218:721–725
De Graauw M (2009) Phospho-proteomics, Methods and Protocols. Humana Press, New York
Ishiwata T, Ishijima C, Ohashi A, Okada H, Ohashi K (2007) Anal Sci 23:755–758
Kittlaus S, Lipinski J, Speer K (2009) J AOAC Int 92:703–714
Pinkse MWH, Heck AJR (2006) Drug Discov Today Tech 3:331–337
Thingholm TE, Jensen ON, Larsen MR (2009) Proteomics 9:1451–1468
Dunn JD, Reid GE, Bruening ML (2010) Mass Spectrom Rev 29:29–54
Larsen MR, Thingholm TE, Jensen ON, Roepstorff P, Jorgensen TJ (2005) Mol Cell Proteomics 4:873–886
Thingholm TE, Jørgensen TJD, Jensen ON, Larsen MR (2006) Nat Protoc 1:1929–1935
Ikeguchi Y, Nakamura H (2000) Anal Sci 16:541–543
Kuroda I, Shintani Y, Motokawa M, Abe S, Furuno M (2004) Anal Sci 20:1313–1319
Sano A, Nakamura H (2004) Anal Sci 20:565–566
Sekiguchi Y, Mitsuhashi N, Inoue Y, Yagisawa H, Mimura T (2004) J Chromatogr A 1039:71–76
Hata K, Morisaka H, Hara K, Mima J, Yumoto N, Tatsu Y, Furuno M, Ishizuka N, Ueda M (2006) Anal Biochem 350:292–297
Aprilita NH, Huck CW, Bakry R, Feuerstein I, Stecher G, Morandell S, Huang H, Stasyk T, Huber LA, Bonn GK (2005) J Proteome Res 4:2312–2319
Josic D, Clifton JG (2007) J Chromatogr A 1144:2–13
Feng S, Pan C, Jiang X, Xu S, Zhou H, Ye M, Zou H (2007) Proteomics 7:351–360
Hou C, Ma J, Tao D, Shan Y, Liang Z, Zhang L, Zhang Y (2010) J Proteome Res 9:4093–4101
Nakanishi K (1997) J Porous Mater 4:67–112
Guiochon G (2007) J Chromatogr A 1168:101–168
Miyazaki S, Morisato K, Ishizuka N, Minakuchi H, Shintani Y, Furuno M, Nakanishi K (2004) J Chromatogr A 1043:19–25
Miyazaki S, Miah MY, Morisato K, Shintani Y, Kuroha T, Nakanishi K (2005) J Sep Sci 28:39–44
Randon J, Huguet S, Demesmay C, Berthod A (2010) J Chromatogr A 1217:1496–1500
Fujita K, Konishi J, Nakanishi K, Hirao K (2004) Appl Phys Lett 85:5595–5597
Nakanishi K (2006) Bull Chem Soc Jpn 79:673–691
Konishi J, Fujita K, Nakanishi K, Hirao K (2006) Chem Mater 18:864–866
Chen Y, Yi Y, Brennan JD, Brook MA (2006) Chem Mater 18:5326–5335
Konishi J, Fujita K, Nakanishi K, Hirao K (2006) Chem Mater 18:6069–6074
Backlund S, Smått JH, Rosenholm JB, Lindén M (2007) J Disper Sci Technol 28:115–119
Konishi J, Fujita K, Nakanishi K, Hirao K, Morisato K, Miyazaki S, Ohira M (2009) J Chromatogr A 1216:7375–7383
Hasegawa G, Kanamori K, Nakanishi K, Hanada T (2010) J Sol-Gel Sci Techno 153:59–66
Hasegawa G, Kanamori K, Nakanishi K, Hanada T (2010) J Am Ceram Soc 93:3110–3115
Zhao J, Jiang ZT, Tan J, Li R (2011) J Sol-Gel Sci Technol 58:436–441
Abi Jaoudé M, Randon J (2011) Anal Bioanal Chem 400:1241–1249
Wang C, Ying JY (1999) Chem Mater 11:3113–3120
Kjellander R, Florin E (1981) J Chem Soc Faraday Trans 1(77):2053–2077
Dormidontova EE (2002) Macromolecules 35:987–1001
Lee Penn R, Banfield JF (1999) Geochim Cosmochim Ac 63:1549–1557
Scherer GW (1988) J Non-Cryst Solids 100:77–92
Scherer GW (1990) J Am Ceram Soc 73:3–14
Gaweł B, Gaweł K, Øye G (2010) Materials 3:2815–2833
Yu JG, Yu HG, Cheng B, Zhao XJ, Yu JC, Ho WK (2003) J Phys Chem B 107:13871–13879
Farneth WE, Kim KS, Barteau MA (1988) Langmuir 4:533–543
Kim JG, Tai WP, Lee KJ, Cho WS (2004) Ceram Int 30:2223–2227
Jaroniec CP, Jaroniec M, Kruk M (1998) J Chromatogr A 797:93–102
Connor PA, McQuillan AJ (1999) Langmuir 15:2916–2921
Brodard-Severac F, Guerrero G, Maquet J, Florian P, Gervais C, Mutin PH (2008) Chem Mater 20:5191–5196
Rob van Veen JA, Veltmaat FTG, Jonkers GJ (1985) Chem Soc, Chem Commun 1656–1658
Sickmann A, Meyer HE (2000) Proteomics 1:200–206
Krebs EG, Beavo JA (1979) Annu Rev Biochem 48:923–959
Krebs EG (1983) Philos Trans Roy Soc B 302:3–11
Hunter T (2000) Cell 100:113–127
Kosik KS, Shimura H (2005) Biochim Biophys Acta 1739:298–310
Yamashita H, Nevalainen MT, Xu J, Le Baron MJ, Wagner K, Erwin RA, Harmon JM, Hennighausen L, Kirken RA, Rui H (2001) Mol Cell Endocrinol 183:151–163
Author information
Authors and Affiliations
Corresponding author
Additional information
Published in the special issue Euroanalysis XVI (The European Conference on Analytical Chemistry) with guest editor Slavica Ražić.
Electronic supplementary material
Below is the link to the electronic supplementary material.
ESM 1
(PDF 197 kb)
Rights and permissions
About this article
Cite this article
Abi Jaoudé, M., Randon, J., Bordes, C. et al. A design of experiment approach to the sol–gel synthesis of titania monoliths for chromatographic applications. Anal Bioanal Chem 403, 1145–1155 (2012). https://doi.org/10.1007/s00216-012-5761-9
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00216-012-5761-9