Abstract
An ultrasound-assisted emulsification microextraction with solidification of organic droplet method followed by high-performance liquid chromatography with diode array detection for six triazole fungicide determination (diniconazole, fluquinconazole, flusilazole, myclobutanil, tebuconazole, and tetraconazole) was developed. After some preliminary experiments, undecanol was chosen as extracting solvent using 50 μL for 10 mL of liquid sample. A central composite design was performed to obtain the best experimental conditions for the following variables NaCl concentration (250 g L−1), extraction time (18 min), and temperature (30 °C) in ultrasonic bath. After the ultrasound-assisted extraction, two steps considering centrifugation (4,200 rpm, 10 min) and solidification (5 min, 3 °C) were done. Following these conditions, the method showed linearity higher than 0.9930 with the concentration ranged from 20 to 890 μg L−1. The limits of detection obtained using calibration curves were from 10.9 to 17.2 μg L−1 and the intra- and inter-day repeatability at two levels showed RSD values between 1.9 and 10.6 %. The enrichment factors for the studied triazoles were between 226 (flusilazole) and 255 (tebuconazole). Recovery studies at two spiked levels in apple and grape juices gave values from 64 to 112 %.
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Acknowledgments
Authors are grateful to the University of Basque Country (UPV/EHU) for financial support (pre-doctoral fellowship for A. B. and EHU 13/52 project).
Compliance with Ethics Requirements
This article does not contain any studies with human or animal subjects.
Conflict of Interest
Ane Bordagaray has no conflict of interest. Rosa Garcia-Arrona has no conflict of interest. Esmeralda Millán has no conflict of interest.
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Bordagaray, A., Garcia-Arrona, R. & Millán, E. Determination of Triazole Fungicides in Liquid Samples Using Ultrasound-Assisted Emulsification Microextraction with Solidification of Floating Organic Droplet Followed by High-Performance Liquid Chromatography. Food Anal. Methods 7, 1195–1203 (2014). https://doi.org/10.1007/s12161-013-9733-2
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DOI: https://doi.org/10.1007/s12161-013-9733-2