Determination of Triazine and Phenylurea Herbicides in Milk Samples Using Ionic Liquid Vortex-assisted Surfactant-enhanced Emulsification Microextraction
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Abstract:
An ionic liquid vortex-assisted surfactant enhanced emulsification microextraction (IL-VASEME) procedure was developed and validated to determine the levels of triazine and phenylurea herbicides in milk using high-performance liquid chromatography (HPLC). 1-Hexyl-3-methylimidazolium hexafluorophosphate (C6MIMPF6) was used as the extraction solvent and was dispersed in the milk solution samples with a vortex. Meanwhile, a surfactant, used as the emulsifier, enhanced the speed of the mass-transfer of analytes from the aqueous phase to the IL and prevented the IL from sticking to the centrifuge tube wall. Acetic acid and Na2SO4 were used to remove proteins and fats, thus eliminating the interference with the analytes. Additionally, the effects of the type and volume of IL, type and concentration of the surfactant, vortex extraction and centrifugation time, ion pair concentration, and sample pH on the extraction efficiency were investigated. Under the optimal conditions, a good linearity was found in the range of 1–400 μg/L, and the correlation coefficients ranged from 0.9963 to 0.9998. The limit of detections (LODs) (0.018–0.095 μg/L) and limit of quantifications (LOQs) (0.10–0.38 μg/L) of the method were calculated based on the signal-to-noise ratios of three and ten of the lowest extractable concentration, respectively. The proposed method was used to determine six herbicides in low fat milk, pasteurized plain milk, pure milk, and fresh milk, and the recovery experiments were performed at three concentration levels, while the recoveries and relative standard deviations (RSDs) ranged from 70.34% to 100.02% and from 2.06% to 9.95%, respectively.
