http://dx.doi.org/10.4322/sc.2016.035
Separation of steroids by temperature-programmed capillary liquid chromatography using packed fused-silica column
Monteiroa, Alessandra Maffei; Coutinhoa, Lincoln Figueira Marins; Nazariob, Carlos Eduardo Domingues; Lanças, Fernando Mauro
Palavras-chave: capillary liquid chromatography, temperature programming, steroids.
Resumo: The miniaturization of liquid chromatography and the development of fused silica capillary packed columns have enable a fast and homogeneous heat transmission through the analytical column. Thus, the use of temperature programming instead of gradient of mobile phase becomes an alternative to decrease the analysis time. This manuscript reports on the applicability of an analytical method for the separation of five steroids by temperature programming capillary liquid chromatography. The influence of the temperature on analytes retention time was investigated and discussed. The steroids were separated by a lab-made capillary column (RP-18) under isocratic elution. The temperature programming allowed to reduce twice the analysis time and diminished the band broadening of the most retained compound in comparison with isothermal analysis.
Referências Bibliográficas
[1] Gritti F. Combined solvent- and non-uniform temperature-programmed gradient liquid chromatography I- A theoretical investigation. J Chromatogr A. 2016; in press; doi:10.1016/j.chroma.2016.09.026.
[2] Wilson RE, Groskreutz SR, Weber SG. Improving the Sensitivity, Resolution, and Peak Capacity of Gradient Elution in Capillary Liquid Chromatography with Large-Volume Injections by Using Temperature-Assisted On-Column Solute Focusing. Anal Chem. 2016;88(10):5112–21.
[3] Weed A-MK, Dvornik J, Stefancin JJ, Gyapong AA, Svec F, Zajickova Z. Photopolymerized organo-silica hybrid monolithic columns: Characterization of their performance in capillary liquid chromatography. J Sep Sci. 2013;36(2):270–8.
[4] Fanali C, Dugo L, Dugo P, Mondello L. Capillary-liquid chromatography (CLC) and nano-LC in food analysis. Trends Anal Chem. 2013;52(0):226–38.
[5] Strain HH. Conditions affecting the sequence of organic compounds in tswett adsorption columns. Ind Eng Chem. 1946;18(10):605–9.
[6] Hesse G, Engelhardt H. Temperaturprogrammierung bei der adsorptionschromatographie von lösungen. J Chromatogr A. 1966;21(C):228–38.
[7] Takeuchi T, Watanabe Y, Ishii D. Role of column temperature in micro high performance liquid chromatography. J High Resolut Chromatogr. 1981;4(6):300–2.
[8] Thompson JD, Carr PW. A study of the critical criteria for analyte stability in high-temperature liquid chromatography. Anal Chem. 2002;74(5):1017–23.
[9] Wiese S, Teutenberg T, Schmidt TC. General Strategy for Performing Temperature Programming in High Performance Liquid Chromatography: Prediction of Linear Temperature Gradients. Anal Chem. 2011;83(6):2227–33.
[10] Sanagi MM, See HH, Ibrahim W, Naim A. High Temperature Liquid Chromatography of Tocol-Derivatives on PolybutadieneCoated Zirconia Stationary Phases. Chromatographia. 2005;61(11–12):567–71.
[11] Groskreutz SR, Horner AR, Weber SG. Temperature-based on-column solute focusing in capillary liquid chromatography reduces peak broadening from pre-column dispersion and volume overload when used alone or with solvent-based focusing. J Chromatogr A. 2015;1405:133–9.
[12] Vanhoenacker G, Sandra P. Elevated temperature and temperature programming in conventional liquid chromatography – Fundamentals and applications. J Sep Sci. 2006;29(12):1822–35.
[13] Greibrokk T, Andersen T. Temperature programming in liquid chromatography. J Sep Sci. 2001;24(12):899–909.
[14] Holland BJ, Conlan XA, Francis PS, Barnett NW, Stevenson PG. Overcoming solvent mismatch limitations in 2D-HPLC with temperature programming of isocratic mobile phases. Anal Methods. 2016;8(6):1293–8.
[15] Cheruthazhekatt S, Harding GW, Pasch H. Comprehensive high temperature two-dimensional liquid chromatography combined with high temperature gradient chromatography-infrared spectroscopy for the analysis of impact polypropylene copolymers. J Chromatogr A. 2013;1286:69–82.
[16] Jensen DS, Teutenberg T, Clark J, Linford MR. Elevated temperatures in liquid chromatography, Part I: Benefits and practical considerations. LCGC North Am. 2012;30(9):850–62.
[17] Guillarme D, Rudaz S, Schelling C, Dreux M, Veuthey JL. Micro liquid chromatography coupled with evaporative light scattering detector at ambient and high temperature: Optimization of the nebulization cell geometry. J Chromatogr A. 2008;1192(1):103–12.
[18] Al-Khateeb L, Smith R. High-temperature liquid chromatography of steroids on a bonded hybrid column. Anal Bioanal Chem. 2009;394(5):1255–60.
[19] Coutinho LFM, Nazario CED, Monteiro AM, Lanças FM. Novel devices for solvent delivery and temperature programming designed for capillary liquid chromatography. J Sep Sci. 2014;37(15):1903–10.
[20] Lanças FM, Rodrigues JC, de S. Freitas S. Preparation and use of packed capillary columns in chromatographic and related techniques. J Sep Sci. 2004;27(17–18):1475–82.
[21] Jensen DS, Teutenberg T, Clark J, Linford MR. Elevated temperatures in liquid chromatography, part III: A closer look at the van ’t Hoff equation. LCGC North Am. 2012;30(12):1052–7.
