Evaluation of α- and β-Endosulfan Residues in Teas and Yerba Mate Infusions by Bar Adsorptive Microextraction and Large Volume Injection-Gas Chromatography Mass Spectrometry

Anaí Dos Santos,José Nogueira,Elina Caramão,Laiza Krause,Jaderson Schneider

doi:10.21577/0103-5053.20190216

Abstract

Tea and yerba mate are traditional beverages prepared through the infusion of leaves of Camellia sinensis and Ilex paraguariensis, respectively. During this process, the leaching of pesticides onto the beverage, such as endosulfan, may occur. In this study, a bar adsorptive microextraction (BAµE) method prior to large gas chromatography mass spectrometry analysis was developed to analyze a- and b-endosulfan in teas and yerba mate infusions. Different sorbent coatings for BAµE were compared and the hydrophilic-lipophilic balanced polymer showed the best selectivity for endosulfan isomers. The method was validated providing good recoveries (varying from 80.4 ± 1.8 to 108 ± 4.9%) and linearities (r2 > 0.99), limits of detection from 8.0 to 4.0 µg kg-1 and limits of quantification from 40 to 20 µg kg-1 for a- and b-endosulfan, respectively. The application of the method in the analysis of real samples showed all free of endosulfan at the limit of detection of the analytical method.

Highlights

Endosulfan is a broad-spectrum organochlorine insecticide and acaricide
This study aims to evaluate the performance of BAμE, as well as the established extraction method stir bar sorptive extraction (SBSE) for α- and β-endosulfan extraction from tea and yerba mate infusions
The results demonstrated the potential of developed BAμE(HLB)/LVI-GC-MS(SIM) method for analysis endosulfan isomers in tea infusion samples at trace level

Summary

Introduction

Endosulfan is a broad-spectrum organochlorine insecticide and acaricide. Its technical grade is a mixture of the two stereoisomers, α- and β-endosulfan, in approximately 2:1 to 7:3 ratio, respectively.[1]. Despite a large number of countries and the European Union having already banned the use of endosulfan,[5]. Different regions have created regulations and set maximum residue levels (MRLs) for endosulfan in tea. The Japan’s Ministry of Health, Labour, and Welfare has established 30 mg kg−1 as the MRL for endosulfan (as a sum of α- and β-endosulfan),[9] while the European Communities Regulation[10] has set the same MRLs value, it is the sum of the isomers and endosulfan sulfate, their major metabolite.[1]

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Conclusion