Repeatability Of Octadecyl Methacrylate-based Monolithic Columns For Capillary Electrochromatography

Octadecyl methacrylate-based monolithic capillary columns were prepared using octadecyl methacrylate as the monomer, ethylene dimethacrylate as the cross-linking agent, 2-acryloylamido-2-methylpropanesulfonic acid as the ionizable monomer, responsible for a negatively charged stationary phase surface and able to support a cathodic electrosmotic flow, and amyl alcohol and 1,4-butanediol as porogenic solvents. The repeatability of the morphological aspect of the monolithic material was evaluated by scanning electron microscopy (SEM). The uniformity along the same monolithic bed was also investigated by SEM. Replicate determinations of surface area and pore volume were also performed and compared. The repeatability of the obtained electrochromatographic efficiencies for separations of alkylbenzenes using the stationary phases prepared was also evaluated. A column that had a plate height of 31 μm was tested for separation of polycyclic aromatic hydrocarbons. Even though minimal possible variation of experimental parameters was maintained, it was not possible to reproduce the stationary phases of the monolithic columns, since the relative standard deviation for the efficiencies obtained on columns prepared from the same polymerization mixture composition was 62%. The lack of repeatability for the efficiency is thought to be a result of limited homogeneity of the monolithic globular structures along the length of the majority of the prepared columns. The poor precision of preparation was justified by the copolymerization reaction that occurs in the presence of 2, 2′-azobisisobutyronitrile as the initiator agent, whose decomposition starts at the moment that this is added to the reaction mixture.432139155Tang, Q., Lee, M.L., Column Technology for Capillary Electrochromatography (2000) Trends Anal. 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A, 1217, pp. 5737-5740Bernabé-Zafón, V., Cantó-Mirapeix, A., Simó-Alfonso, E.F., Ramis-Ramos, G., Herrero-Martínez, J.M., Comparison of Thermal and Photo Polymerization of Lauryl Methacrylate Monolithic Columns for CEC (2009) Electrophoresis, 30, pp. 1929-1936Kositarat, S., Smith, N.W., Nacapricha, D., Wilairat, P., Chaisuwan, P., Repeatability in Column Preparation of a Reversed-phase C18 Monolith and its Application to Separation of Tocopherol Homologues (2011) Talanta, 84, pp. 1374-1378Nischang, I., Teasdale, I., Brüggemann, O., Towards Porous Polymer Monoliths for the Efficient, Retention-independent Performance in the Isocratic Separation of Small Molecules by Means of Nano-liquid Chromatography (2010) J. Chromatogr. A, 1217, pp. 7514-7522Ludewig, R., Nietzsche, S., Scriba, G.K.E., A Weak Cation-exchange Monolith as Stationary Phase for the Separation of Peptide Diastereomers by CEC (2011) J. Sep. Sci., 34, pp. 64-69Yamada, H., Kitagawa, S., Ohtani, H., Simultaneous Separation of Water- and Fat-soluble Vitamins in Isocratic Pressure-assisted Capillary Electrochromatography Using a Methacrylate-based Monolithic Column (2013) J. Sep. Sci., 36, pp. 1980-1985Geiser, L., Eeltink, S., Svec, F., Fréchet, J.M.J., Stability and Repeatability of Capillary Columns Based on Porous Monoliths of Poly(butyl methacrylate-co-ethylene dimethacrylate) (2007) J. Chromatogr. A, 1140, pp. 140-146Nischang, I., Svec, F., Fréchet, J.M.J., Effect of Capillary Cross-section Geometry and Size on the Separation of Proteins in Gradient Mode Using Monolithic Poly(butyl methacrylate-co-ethylene dimethacrylate) Columns (2009) J. Chromatogr. A, 1216, pp. 2355-2361Deyl, Z., Svec, F., (2001) Capillary Electrochromatography, , Elsevier Science B.V.: Berkeley, CASmith, N.W., Jiang, Z., Developments in the Use and Fabrication of Organic Monolithic Phases for Use with High-performance Liquid Chromatography and Capillary Electrochromatography (2008) J. Chromatogr. A, 1184, pp. 416-440Svec, F., Recent Developments in the Field of Monolithic Stationary Phases for Capillary Electrochromatography (2005) J. Sep. Sci., 28, pp. 729-745Urban, J., Svec, F., Fréchet, J.M.J., Hypercrosslinking: New Approach to Porous Polymer Monolithic Capillary Columns of Large Surface Area for the Highly Efficient Separation of Small Molecules (2010) J. Chromatogr. A, 1217, pp. 8212-8221Lubbad, S.H., Buchmeiser, M.R., Fast Separation of Low Molecular Weight Analytes on Structurally Optimized Polymeric Capillary Monoliths (2010) J. Chromatogr. 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Physical And Electrophoretic Characterization Of Octadecyl Methacrylate-based Monolithic Columns For Use In Capillary Electrochromatography

Organic monolithic columns with high efficiency were obtained for use in capillary electrochromatography (CEC) from a mixture of monomers (constant concentrations) with different proportions of porogenic solvents (1,4-butanediol with isoamyl alcohol, amyl alcohol or cyclohexanol in the presence or absence of water). The stationary phases were prepared from the precursor monomer octadecyl methacrylate (ODMA), the cross-linking agent ethylene dimethacrylate (EDMA) and the ionizable monomer 2-acryloylamido-2-methylpropanesulfonic acid (AMPS), the latter being necessary to make the stationary phase negatively charged, assuring electrosmotic flow (EOF) during analysis. The monolithic columns synthesized were physically characterized by porosimetry and scanning electron microscopy (SEM), and electrochromatographically characterized by calculation of chromatographic parameters. 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Chromatographic Evaluation Of Self-immobilized Stationary Phases For Reversed-phase Liquid Chromatography

The preparation of stationary phases for HPLC using polymers deposited on silica usually includes an immobilization step involving cross-linking by free radicals induced by ionizing radiation or by other radical initiators. The present paper reports changes which occur at ambient temperature in the character of poly(methyloctylsiloxane) deposited on porous silica particles as a function of the time interval between particle loading and column packing. Column performance and retention factors increase with time and these changes are attributed to rearrangement (self-assembly) which result in "self-immobilization" of the polymer molecules on the silica surface. © 2002 Elsevier Science B.V. All rights reserved.98701/02/158792Snyder, L.R., Kirkland, J.J., Glajch, J.L., Practical HPLC Method Development (1997), p. 189. , New York: WileyKirkland, J.J., Glajch, J.L., Farlee, R.D., (1989) Anal. Chem., 61, p. 2Pesek, J.J., Matyska, M.T., Sandoval, J.E., Williamsen, E.J., (1996) J. Liq. Chromatogr. Rel. Technol., 19, p. 2843Voort, P.V.D., Vansant, E.F., (1996) J. Liq. Chromatogr. Rel. Technol., 19, p. 2723Buszewski, B., Jezierska, M., Welniak, M., Berek, D., (1998) J. High Resolut. Chromatogr., 21, p. 267Sander, L.C., Pursch, M., Wise, S.A., (1999) Anal. Chem., 71, p. 4821Fairbank, R.W.P., Wirth, M.J., (1999) J. Chromatogr. A, 830, p. 285Hanai, T., (2000) Adv. Chromatogr., 40, p. 315Silva, C.R., Bachmann, S., Schefer, R.R., Albert, K., Jardim, I.C.S.F., Airoldi, C., (2002) J. Chromatogr. A, 948, p. 85Petro, M., Berek, D., (1993) Chromatographia, 37, p. 549Hanson, M., Unger, K.K., (1992) Trends Anal. Chem., 11, p. 368Hanson, M., Kurganov, A., Unger, K.K., Davankov, V.A., (1993) J. Chromatogr. A, 656, p. 369Jardim, I.C.S.F., Collins, K.E., Anazawa, T.A., (1999) J. Chromatogr. A, 849, p. 299Anazawa, T.A., Jardim, I.C.S.F., (1994) J. Liq. Chromatogr., 17, p. 1265Anazawa, T.A., Jardim, I.C.S.F., (1998) J. Liq. Chromatogr. Rel. Technol., 21, p. 645Collins, K.E., Bottoli, C.B.G., Bachmann, S., Vigna, C.R.M., Collins, C.H., Albert, K., Chem. Mater., , in pressCollins, K.E., Franchon, A.C., Jardim, I.C.S.F., Radovanovic, E., Gonçalves, M.C., (2000) LC·GC, 18, p. 106Collins, K.E., Sá, A.L.A., Bottoli, C.B.G., Collins, C.H., (2001) Chromatographia, 53, p. 661Collins, K.E., Granja, M.L.M.M., Pereira Filho, R.G., Anazawa, T.A., Jardim, I.C.S.F., (1997) Chromatographia, 45, p. 99Claessens, H.A., Van Straten, M.A., Cramers, C.A., Jezierska, M., Buszewski, B., (1998) J. Chromatogr. A, 826, p. 135Stella, C., Rudaz, S., Veuthey, J.-L., Tchapla, A., (2001) Chromatographia, 53, p. 132Claessens, H.A., (2001) Trends Anal. Chem., 20, p. 563Engelhardt, H., Arangio, M., Lobert, T., (1997) LC·GC, 15, p. 856Walters, M.J., (1987) J. Assoc. Off. Anal. Chem., 70, p. 465Kimata, K., Iwaguchi, K., Onishi, S., Jinno, K., Eksteen, R., Hosoya, K., Araki, M., Tanaka, N., (1989) J. Chromatogr. Sci., 27, p. 72

Nano-liquid Chromatography In Pharmaceutical And Biomedical Research

Miniaturized separation techniques have emerged as environmentally friendly alternatives to available separation methods. Nano-liquid chromatography (nano-LC), microchip devices and nano-capillary electrophoresis are miniaturized methods that minimize reagent consumption and waste generation. Furthermore, the low levels of analytes, especially in biological samples, promote the search for more highly sensitive techniques; coupled to mass spectrometry, nano-LC has great potential to become an indispensable tool for routine analysis of biomolecules. This short review presents the fundamental aspects of nano-LC analytical instrumentation, discussing practical considerations and the primary differences between miniaturized and conventional instrumentation. Some theoretical aspects are discussed to better explain both the potential and the principal limitations of nano-LC. 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Possibilities And Limitations Of Using Temperature In Reversed Phase Liquid Chromatography [possibilidades E Limitações No Uso Da Temperatura Em Cromatografia Líquida De Fase Reversa]

High-temperature liquid chromatography (HTLC) is a technique that presents a series of advantages in liquid phase separations, such as: reduced analysis time, reduced pressure drop, reduced asymmetry factors, modified retentions, controlled selectivities, better efficiencies and improved detectivities, as well as permitting green chromatography. The practical limitations that relate to instrumentation and to stationary phase instability are being resolved and this technique is now ready to be applied for routine determinations.334945953Antia, F.D., Horvath, Cs., (1988) J. Chromatogr., 435, p. 1Yang, B., Zhao, J., Brown, J.S., Blackwell, J., Carr, P.W., (2000) Anal. Chem., 72, p. 125Guillarme, D., Heinisch, S., Rocca, J.L., (2004) J. Chromatogr. A, 1052, p. 39Petersson, P., Euerby, M.R., (2007) J. Sep. Sci., 30, p. 2012Sandra, P., Vanhoenacker, G., (2007) J. Sep. Sci., 30, p. 241Edge, A.M., Shillingford, S., Smith, C., Payne, R., Wilson, I.D., (2006) J. Chromatogr. 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Preparation Of Stationary Phases For Reversed-phase High-performance Liquid Chromatography Using Thermal Treatments At High Temperature

Batches of poly(methyloctylsiloxane) (PMOS)-loaded silica were prepared by deposition from a solution of PMOS into the pores of HPLC silica. Portions of PMOS-loaded silica were subjected to a thermal treatment at 100 °C for 24 h (condition 1) in a tube furnace under a nitrogen atmosphere. After that, the material was heated for 4 h at higher temperatures (150-400 °C) (condition 2). Heating at higher temperatures produces polymer bilayers. Non-immobilized and thermally treated stationary phases were characterized by percent carbon, 29Si cross-polarization magic angle spinning nuclear magnetic resonance spectroscopy and reversed-phase chromatographic performance. The results show that thermal treatment between 150 and 300 °C accelerates the immobilization process, possibly due to some bond breaking of the polysiloxane, with formation of strong linkages to the surface of the support, resulting in more complete coverage of the silica. The chromatographic results show an improvement of efficiency with the increase of the temperature of condition 2 up to 300 °C and an increase in the resolution of the components, mainly for the phase heated at 300 °C. Such results demonstrate that a two-step thermal treatment (100 °C then 150-300 °C) produces stationary phases with good properties for use in reversed-phase high-performance liquid chromatography. © 2007 Elsevier B.V. All rights reserved.11561-2 SPEC. ISS.6067Schomburg, G., (1991) Trends Anal. Chem., 10, p. 163Petro, M., Berek, D., (1993) Chromatographia, 37, p. 549Jardim, I.C.S.F., Collins, K.E., Collins, C.H., (2004) Microchem. J., 77, p. 191Anazawa, T.A., Jardim, I.C.S.F., (1994) J. Liq. Chromatogr., 17, p. 1265Collins, K.E., Granja, M.L.M.M., Pereira, R.G., Anazawa, T.A., Jardim, I.C.S.F., (1997) Chromatographia, 45, p. 99Mano, E.B., Mendes, L.C., (1999) Introdução a Polímeros. second revised ed., , Edgard Blücher, São PauloPetsev, N.D., Perov, G.I., Alexandrova, M.D., (1985) Chi. Dimitov, Chromatographia, 20, p. 228Gawdizik, J., (1991) Chromatographia, 31, p. 258Bemgard, A., Blomberg, L.G., (1987) J. Chromatogr., 395, p. 125Chuang, C.H., Shanfield, H., Zlatkis, A., (1987) Chromatographia, 23, p. 169Markides, K., Blomberg, L., Buijten, J., Wännman, T., (1983) J. Chromatogr., 267, p. 29Schomburg, G., Köhler, J., Figge, H., Deege, A., Bien-Vogelsang, U., (1984) Chromatographia, 18, p. 265Jardim, I.C.S.F., Collins, K.E., Anazawa, T.A., (1999) J. Chromatogr. A, 849, p. 299Bottoli, C.B.G., Vigna, C.R.M., Fischer, G., Albert, K., Collins, K.E., Collins, C.H., (2004) J. Chromatogr., 1030, p. 217Bottoli, C.B.G., Collins, K.E., Collins, C.H., (2003) J. Chromatogr. A, 987, p. 87Collins, K.E., Bottoli, C.B.G., Vigna, C.R.M., Bachmann, S., Albert, K., Collins, C.H., (2004) J. Chromatogr. A, 1029, p. 43Morais, L.S.R., Jardim, I.C.S.F., (2005) J. Chromatogr. A, 1073, p. 127Lopes, N.P., Collins, K.E., Jardim, I.C.S.F., (2003) J. Chromatogr. A, 987, p. 77Tonhi, E., Collins, K.E., Collins, C.H., (2005) J. Chromatogr. A, 1075, p. 87Faria, A.M., Collins, K.E., Collins, C.H., (2006) J. Chromatogr. A, 1122, p. 114Pozzebon, J.M., Queiroz, S.C.N., Melo, L.F.C., Kapor, M.A., Jardim, I.C.S.F., (2003) J. Chromatogr. A, 987, p. 381Ohmacht, R., Kele, M., Matus, Z., (1989) Chromatographia, 28, p. 19Collins, K.E., Sá, A.L.A., Bottoli, C.B.G., Collins, C.H., (2001) Chromatographia, 53, p. 661Bottoli, C.B.G., Chaudhry, Z.F., Fonseca, D.A., Collins, K.E., Collins, C.H., (2002) J. Chromatogr. A, 948, p. 121Collins, K.E., Franchon, A.C., Jardim, I.C.S.F., Radovanovic, E., Gonçalves, M.C., (2000) LC-GC, 18, p. 106Bachmann, S., Melo, L.F.C., Silva, R.B., Anazawa, T.A., Jardim, I.C.S.F., Collins, K.E., Collins, C.H., Albert, K., (2001) Chem. Mater., 13, p. 1874Snyder, L.R., Kirkland, J.J., (1979) Introduction to Modern Liquid Chromatography. second ed., , Wiley, New YorkLopes, N.P., Collins, K.E., Jardim, I.C.S.F., (2004) J. Chromatogr. A, 1030, p. 225Nawrocki, J., (1991) Chromatographia, 31, p. 177Kirkland, J.J., Boyes, B.E., DeStefano, J.J., (1994) Am. Lab., 26, p. 3

Application Of Genetic Algorithm For Selection Of Variables For The Blls Method Applied To Determination Of Pesticides And Metabolites In Wine

A variable selection methodology based on genetic algorithm (GA) was applied in a bilinear least squares model (BLLS) with second-order advantage, in three distinct situations, for determination by HPLC-DAD of the pesticides carbaryl (CBL), methyl thiophanate (TIO), simazin (SIM) and dimethoate (DMT) and the metabolite phthalimide (PTA) in wine. The chromatographic separation was carried out using an isocratic elution with 50:50 (v/v) acetonitrile:water as mobile phase. Preprocessing methods were performed for correcting the chromatographic time shifts, baseline variation and background. The optimization by GA provided a significant reduction of the errors, where for SIM and PTA a decrease of three times the value obtained using all variables, and an improvement in the distribution of them, reducing the observed bias in the results were observed. Comparing the RMSEP of the optimized model with the uncertainty estimates of the reference values it is observed that GA can be a very useful tool in second-order models. © 2006 Elsevier B.V. All rights reserved.5951-2 SPEC. ISS.5158Forrest, S., (1993) Science, 261, p. 872Goldberg, D.E., (1989) Genetic Algorithm in Search, Optimization and Machine Learning, , Addison-Wesley, New York p. 125Bangalore, A.S., Shaffer, R.E., Small, G.W., Arnold, M.A., (1996) Anal. Chem., 68, p. 4200Ding, Q., Smal, G.W., Arnold, M.A., (1998) Anal. Chem., 70, p. 4472Costa Filho, P.A., Poppi, R.J., (2001) Anal. Chim. Acta, 446, p. 39Lomillo, M.A.A., Renedo, O., Martinéz, M.J.A., (2001) Anal. Chim. Acta, 449, p. 167Ghasemi, J., Niazi, A., Leardi, R., (2003) Talanta, 59, p. 311Abdollahi, A., Bagheri, L., (2004) Anal. Chim. Acta, 514, p. 211Dantas Filho, H.A., Souza, E.S.O.N., Visani, V., Barros, S.R.R.C., Saldanha, T.C.B., Araújo, M.C.U., Galvão, R.K.H., (2005) J. Braz. Chem. Soc., 16, p. 58Ghasemi, J., Ebrahimi, D.M., Hejazi, L., Leardi, R., Niazi, A., (2006) J. Anal. Chem., 61, p. 92Franco, V.G., Perin, J.C., Mantovani, V.E., Goicoechea, H.C., (2006) Talanta, 68, p. 1005Wu, W., Guo, Q., Massart, D.L., Boucon, C., de Jong, S., (2003) Chemometr. Intell. Lab. Syst., 65, p. 83Lopes, J.A., Menezes, J.C., (2003) Chemometr. Intell. Lab. Syst., 68, p. 75Gourvénec, S., Capron, X., Massart, D.L., (2004) Anal. Chim. Acta, 519, p. 11Linder, M., Sundberg, R., (1998) Chemometr. Intell. Lab. Syst., 42, p. 159Linder, M., Sundberg, R., (2002) J. Chemometr., 16, p. 12Damiani, P.C., Nepote, A.J., Bearzotti, M., Olivieri, A.C., (2004) Anal. Chem., 76, p. 2798Marsili, N.R., Lista, A., Band, B.S.F., Goicoechea, H.C., Olivieri, A.C., (2005) Analyst, 130, p. 1291Goicoechea, H.C., Olivieri, A.C., (2005) Appl. Spectrosc., 59, p. 926Haimovich, A., Orselli, R., Escandar, G.M., Olivieri, A.C., (2006) Chemometr. Intell. Lab. Syst., 80, p. 99Faber, N.M., Ferré, J., Boqué, R., Kalivas, J.H., (2002) Chemometr. Intell. Lab. Syst., 63, p. 107Öhman, J., Geladi, P., Wold, S., (1990) J. Chemometr., 4, p. 79Lorber, A., (1986) Anal. Chem., 58, p. 1167Messick, N.J., Kalivas, J.H., Lang, P.M., (1996) Anal. Chem., 68, p. 1572Ho, C.N., Christian, G.D., Davidson, E.R., (1980) Anal. Chem., 52, p. 1071Olivieri, A.C., Faber, N.M., (2005) J. Chemometr., 19, p. 583Boqué, R., Larrechi, M.S., Rius, F.X., (1999) Chemometr. Intell. Lab. Syst., 45, p. 397Boqué, R., Ferre, J., Faber, N.M., Rius, F.X., (2002) Anal. Chim. Acta, 451, p. 313Olivieri, A.C., Faber, N.M., (2004) Chemometr. Intell. Lab. Syst., 70, p. 75Miller-Ihli, N.J., O'Haver, T.C., (1984) Spectrochim. Acta, 39 B, p. 1603http://www.codexalimentarius.net/mrls/pestdes/jsp/pest_q-e.jspPrazen, B.J., Synovec, R.E., Kowalski, B.R., (1998) Anal. Chem., 70, p. 218Riu, J., Rius, F.X., (1996) Anal. Chem., 68, p. 185

Volatile Organic Contaminants From Plastic Packaging: Development And Validation Of Analytical Methods [contaminantes Voláteis Provenientes De Embalagens Plásticas: Desenvolvimento E Validação De Métodos Analíticos]

Plastic packaging materials intended for use in food packaging is an area of great interest from the scientific and economic point of view due to the irreversible internationalization and globalization process of food products. Nevertheless, a debate related to food safety aspects has emerged within the scientific community. Therefore, the development of analytical methods that allow identifying and quantifying chemical substances of toxicological potential in the packaging is considered essential. This article focuses on the main analytical methods, including validation parameters, as well as extraction and quantification techniques for determination of volatile organic compounds from food packaging materials.31615221532Rundh, B., (2005) Br. Food J, 107, p. 670Arvanitoyannis, I., Bosnea, L., (2001) Food Rev. Int, 17, p. 291Ahmed, A., Ahmed, N., Salman, A., (2005) Br. 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Monolithic Stationary Phases For Chromatographic Separations [fases Estacionárias Monolíticas Para Separações Cromatográficas]

Monolithic stationary phases represent a new generation of Chromatographic separation media. These phases consist of a continuous separation bed prepared by in situ polymerization or consolidation inside the column tubing. In recent years, their simple preparation procedure, unique properties and excellent performance have attracted quite remarkable attention in liquid chromatography and capillary electrochromatography. This review summarizes the preparation, characterization and applications of monolithic stationary phases. The analytical potential of these columns is demonstrated with separations involving various families of compounds in different separation modes.292300309Svec, F., Peters, E.C., Sýkora, D., Fréchet, J.M.J., (2000) J. Chromatogr., A, 887, p. 3Tanaka, N., Kobayashi, H., (2003) Anal. Bioanal. Chem., 376, p. 298Zou, H., Huang, X., Ye, M., Luo, Q., (2002) J. Chromatogr., A, 954, p. 5MacNair, J.E., Patel, K.D., Jorgenson, J.W., (1999) Anal. 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