Development and validation of analytical methodologies for determination of pesticides in the cultivation of cucumbers, using ultra performance liquid chromatograph

Author(s)

Luana Cristina Macedo

• Document type: Master's Dissertation
• Press: Campinas, SP.
• Institution: Universidade Estadual de Campinas (UNICAMP). Instituto de Química
• Defense date: 2014-05-14

Examining board members

Isabel Cristina Sales Fontes Jardim; Bruno José Gonçalves Silva; Dosil Pereira de Jesus

• Advisor: Isabel Cristina Sales Fontes Jardim

Abstract

In developing countries, such as Brazil, impacts to the environment and to the public healthhave increased by the use of different pesticides. In fact, the widely application of these compounds in various cultures is due to increasing of productivity as well as quality. These pesticides are frequently applied without compliance to the recommendations of the Good Agricultural Practices. To increase the production levels and the food quality, pesticides are essential for agriculture, however due to the health risk to the population, the use of some types of pesticides have been banned in some countries, as Brazil. In this context, the QuEChERS extraction method associated with ultra -efficiency liquid chromatography (UHPLC) was developed and evaluated for quantitative analysis and confirmation of 18 pesticides, which are allowed and not allowed in the culture of cucumbers, for purposes of quality control to follow the regulatory agencies guides about accepted maximum residue limits (MRL). First of all, a method based on QuEChERS for sample preparation and liquid chromatography with ultra efficiency diode array detector (UHPLC-DAD) was developed and validated for a multiresidue determination of pesticides in cultivation of cucumber, presenting adequate chromatographic resolution and short analysis time (14 min). Modifications to the method of sample preparation provided acceptable recovery percentagens (70-120%), with coefficients of variation (CV) below 20%, as recommended by the SANCO guide to pesticides evaluated. However, certain limitations, such as low selectivity and sensibility for some compounds, that were found when the DAD detector was used, lead to the use of the mass spectrometer tandem coupled to UHPLC (UHPLC-MS/MS), also employing the method QuEChERS as sample preparation. This method developed and validated showed selectivity, linearity and limits lower than the MRL of each compound quantification established by ANVISA, and it was more selective and sensitive than UHPLC-DAD. Analyses of samples from near local market (Campinas-SP) indicated the presence of pesticide residues allowed and not allowed in cultured cucumbers, proving the value of the proposed study (AU)

• FAPESP's process: 12/01667-6 - Development and validation of analytical methodologies for determination of pesticides in the cultivation of cucumbers, using ultra performance liquid chromatography (UPLC)
• Grantee: Luana Cristina Macedo
• Support Opportunities: Scholarships in Brazil - Master