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Development of silica modified with ionic liquids and their use in sample preparation techniques

Grant number: 12/22055-9
Support type:Scholarships in Brazil - Doctorate
Effective date (Start): March 01, 2013
Effective date (End): February 28, 2017
Field of knowledge:Physical Sciences and Mathematics - Chemistry - Analytical Chemistry
Principal researcher:Fernando Mauro Lanças
Grantee:Meire Ribeiro da Silva
Home Institution: Instituto de Química de São Carlos (IQSC). Universidade de São Paulo (USP). São Carlos , SP, Brazil
Associated scholarship(s):15/12306-2 - Preparation, evaluation and separation optimization of porous-layer open-tubular (PLOT)columns for nano-LC-MS/MS analysis of sulfonamides and their acetylated metabolites in food samples, BE.EP.DR


Antimicrobials are applied to dairy cattle with goal therapeutic, prophylactic and to stimulate growth. Improper use of antimicrobials in dairy cows, particularly sulfonamides, leads to the possibility of residues of these substances in milk. In this context is necessary the use of specific and selective analytical methods in order to achieve the residue limits set by agencies responsible ensuring the quality of the final product. A classical method of quantifying SAs residues in milk is shown by AOAC International, which uses liquid-liquid extraction, and the extracts are analyzed by high performance liquid chromatography (HPLC). Although HPLC presents several advantages such as, high resolution, versatility, amongst others, this in itself does not solve all analytical problems mainly with the increase in the number of residues and contaminants present in complex matrices. Therefore, it is important to use techniques for more efficient sample preparation in order to increase the selectivity. Among the sample preparation techniques stands miniaturized techniques (e.g., a solid phase microextraction (SPME), the solid phase microextraction the tube (in-tube SPME) in the sorptive extraction stirring bar (SBSE) , microextraction by packed sorbent (MEPS), liquid phase microextraction (LPME)) due to lower consumption of solvent, sorbent among other advantages. Currently the use of sorbents for these classical methods of preconcentration have been largely replaced by modified materials such as silica and polymers in order to increase the selectivity. The most recent publications show immobilization of surfaces of various materials such as silica with ILs or polymerizing materials with ILs, that exhibit success as adsorbent materials. Ionic liquids at room temperature (ILs) have been used as "green solvents" to replace traditional organic solvents for chemical reactions. Due to its low stability, high thermal volatility and good solubility for these organic and inorganic. These products have been successfully applied in the field of analytical chemistry, such as extraction liquid-phase liquid-liquid microextraction, solid phase microextraction, electrolyte additives in CE and GC stationary phases. In addition to the advantages of the use of adsorbents with high selectivity when used in preconcentration techniques in hyphenated analytical systems for separation and detection, for obtaining a rapid analysis, low consumption of solvent, lower exposure to toxic solvents analysts, as well as increased analytical accuracy and automation of the analysis. This work will develop a new sorbent (silica surface modified with an ionic liquid) to be applied as sorbent in the sample preparation in online systems such as SPE online and in-tube SPME. The characterization of the synthesized adsorbent will be performed by FT-IR, SEM and BET. Factors optimization of separation and extraction will be evaluated by factorial design. The results of extraction using modified silica IL will be compared with C18 sorbent commercial. The method will be applied for the simultaneous detection of sulfonamides in 10 samples of bovine milk.

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Scientific publications (5)
(References retrieved automatically from Web of Science and SciELO through information on FAPESP grants and their corresponding numbers as mentioned in the publications by the authors)
NAZARIO, CARLOS E. D.; SILVA, MEIRE R.; FRANCO, MARAISSA S.; LANCAS, FERNANDO M.. Evolution in miniaturized column liquid chromatography instrumentation and applications: An overview. Journal of Chromatography A, v. 1421, p. 18-37, . (05/59360-0, 12/22055-9, 14/07347-9)
DOMINGUES NAZARIO, CARLOS EDUARDO; FUMES, BRUNO HENRIQUE; DA SILVA, MEIRE RIBEIRO; LANCAS, FERNANDO MAURO. New materials for sample preparation techniques in bioanalysis. JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES, v. 1043, p. 81-95, . (15/12306-2, 15/15462-5, 12/22055-9, 14/07347-9)
FUMES, BRUNO HENRIQUE; SILVA, MEIRE RIBEIRO; ANDRADE, FELIPE NASCIMENTO; DOMINGUES NAZARIO, CARLOS EDUARDO; LANCAS, FERNANDO MAURO. Recent advances and future trends in new materials for sample preparation. TRAC-TRENDS IN ANALYTICAL CHEMISTRY, v. 71, n. SI, p. 9-25, . (11/09898-4, 12/22055-9, 14/07347-9, 13/17425-4)
SILVA, MEIRE R.; ANDRADE, FELIPE N.; FUMES, BRUNO H.; LANCAS, FERNANDO M.. Unified chromatography: Fundamentals, instrumentation and applications. JOURNAL OF SEPARATION SCIENCE, v. 38, n. 17, p. 3071-3083, . (11/09898-4, 12/22055-9, 14/07347-9, 13/17425-4)
Academic Publications
(References retrieved automatically from State of São Paulo Research Institutions)
SILVA, Meire Ribeiro da. New strategies of sample preparation for determination of sulfonamides in complex matrices. 2017. Doctoral Thesis - Universidade de São Paulo (USP). Instituto de Química de São Carlos (IQSC/BT) São Carlos.

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