Dispersive liquid–liquid microextraction based on the solidification of floating organic droplets for HPLC determination of three strobilurin fungicides in cereals

Abstract

ABSTRACT In this paper, a dispersive liquid–liquid microextraction method based on the solidification of floating organic droplets, combined with high-performance liquid chromatography (DLLME-SFOD-HPLC), was developed for the detection of strobilurin fungicides (azoxystrobin, pyraclostrobin, and trifloxystrobin) in cereals. Natural fatty acids were used as an extractant and have low toxicity, density, and freezing point. The extractant nonanoic acid was evenly dispersed as droplets in sample solution and was then solidified in the upper layer of sample solution after centrifugation and ice bath, which improved the extraction and collection efficiency. The dispersive liquid-liquid microextraction procedure was optimised by univariate analysis and the Box-Behnken response surface methodology. Optimum conditions were as follows: the volume of nonanoic acid was 82 μL, the volume of acetonitrile was 620 μL, and the amount of salt was 256 mg. Under optimised conditions, the method had good linearity with a correlation coefficient higher than 0.997, and the limit of detection was 2.57–4.87 μg kg−1. The recoveries of azoxystrobin, pyraclostrobin, and trifloxystrobin in rice, corn, and wheat were 82.0%-93.2%, and the relative standard deviations were 1.6%-7.4%. Therefore, the method was successfully applied to detect target fungicides in cereals.