Abstract

A novel method for the determination of butachlor and fipronil in liquid milk has been developed using ionic liquid dispersive liquid-liquid microextraction coupled with ultra-high performance liquid chromatography (UHPLC). The optimum extraction conditions were determined to be 60 μL of 1-octyl-3-methyl imidazole six fluorine phosphate extraction solvent, 1000 μL of acetonitrile as the dispersing solvent, vortex extraction time of 3 min, centrifugation for 5 min at room temperature at 10 000 rpm. After extraction, 30 μL of extraction solvent was obtained from the sample for UHPLC analysis. It was shown that good linearity was obtained with butachlor and fipronil concentrations from 5 to 1000 μg/kg with correlation coefficient of 0.999. The average recoveries were in the range of 90 to 104% at spiked levels from 10 to 50 μg/kg with intra-day relative standard deviations lower than 3.7% (n = 6) and inter-day relative standard deviations lower than 6.1% (n = 3). The limits of detection were 0.5 and 0.3 μg/kg for butachlor and fipronil, respectively.

中文翻译：

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离子液体分散液微萃取-超高效液相色谱法测定液态牛奶中的丁草胺和氟虫腈

摘要

离子液体分散液-液微萃取-超高效液相色谱法（UHPLC）建立了测定乳汁中丁草胺和氟虫腈的新方法）。确定最佳提取条件为60μL1-辛基-3-甲基咪唑六氟磷酸提取溶剂，1000μL乙腈作为分散溶剂，涡旋提取时间3分钟，在室温下于10离心5分钟000转/分。提取后，从样品中获得30μL提取溶剂用于UHPLC分析。结果表明，丁草胺和氟虫腈的浓度为5至1000μg/ kg时，具有良好的线性关系，相关系数为0.999。在10到50μg/ kg的加标水平下，平均回收率在90到104％的范围内，日内相对标准偏差低于3.7％（n = 6），日间相对标准偏差低于6.1％（ñ= 3）。丁草胺和氟虫腈的检出限分别为0.5和0.3μg/ kg。