Plant Protection College, Shenyang Agricultural University, Shenyang, China.
Liaoning entry-exit inspection and quarantine bureau, Dalian, China.
J Sep Sci. 2017 Oct;40(19):3882-3888. doi: 10.1002/jssc.201700498. Epub 2017 Aug 31.
A rapid and simple sample preparation method was developed for simultaneous determination of three triazine herbicides in honey samples. The selected herbicides were extracted from honey samples by ionic liquid dispersive liquid-liquid microextraction, separated on a C column (250 mm × 4.6 mm id, 5 μm) using acetonitrile and H O as the mobile phase with gradient elution, and then detected by high-performance liquid chromatography. The parameters, such as the type and volume of the extraction and disperser solvent, ion strength, pH, extraction time, and centrifuge time were optimized in order to provide the excellent extraction performance. Good linearity was showed for all the target herbicides over the tested concentration range with correlation coefficient higher than 0.994. Three spiked levels (0.005, 0.05, 0.10 mg/kg) were applied for determination of the recoveries of the targets in honey samples in the range of 80-103% with relative standard deviations not larger than 10.6%. The limits of quantification for the analytes ranged between 1.5 and 4.0 μg/kg. The developed method was applied for determination of the target compounds residues in real samples.
建立了一种快速、简单的样品前处理方法，用于蜂蜜样品中三种三嗪类除草剂的同时测定。选择的除草剂用离子液体分散液液微萃取从蜂蜜样品中提取，在 C 柱（250mm×4.6mmid，5μm）上用乙腈和 H 2 O 作为流动相进行梯度洗脱，然后用高效液相色谱法检测。优化了萃取和分散溶剂的类型和体积、离子强度、pH 值、萃取时间和离心时间等参数，以提供优异的萃取性能。所有目标除草剂在测试浓度范围内均表现出良好的线性，相关系数均高于 0.994。在蜂蜜样品中，以 0.005、0.05 和 0.10mg/kg 三个加标水平进行测定，目标物的回收率在 80-103%范围内，相对标准偏差不大于 10.6%。分析物的定量限在 1.5 和 4.0μg/kg 之间。该方法已应用于实际样品中目标化合物残留量的测定。
