摘要
将沉积固化离子液体均相液液微萃取与高效液相色谱相结合,建立同时测定蔬菜中残留的异丙隆、灭草隆、敌草隆、绿麦隆和绿谷隆5种苯脲类除草剂的分析方法,选用三丁基辛基溴化膦([P4448]Br)为萃取剂,样品溶液经水浴和超声后,加入离子对试剂,使之发生原位反应,经冰浴和离心后,富集有目标物的离子液体与样品溶液实现相分离,并沉积在离心管底部,取离子液体部分进行色谱分析。在单因素试验基础上,采用Box-Behnken响应面试验设计对主要萃取条件进行优化。结果表明,各目标物回归模型失拟项均不显著(P>0.05),校正相关系数R2大于0.91,模型较好,拟合度较高。各化合物在线性关系内具有良好的线性关系(r≥0.9981),检出限和定量限分别为2.19~5.35μg/kg和7.30~17.82μg/kg,加标回收率在82.84%~117.49%之间。该方法溶剂用量少、绿色环保、操作简单,可用于蔬菜中苯脲类农药残留的分析与检测。
In this study,an analytical method using homogeneous liquid-liquid microextraction based on the solidification of sedimentary ionic liquid coupled with high performance liquid chromatography(HPLC)was developed and applied to the simultaneous determination of five phenylurea pesticide residues in vegetables.The hydrophilic ionic liquid noctyltributylphosphonium bromide([P4448]Br)was used as the microextraction solvent.The extraction was carried out with the aid of ultrasound,after centrifugation and cooling.The analytes were enriched into the ionic liquid phase and deposited at the bottom of the centrifuge tube.The ionic liquid phase was diluted and used for chromatographic analysis.The combined use of one-factor-at-a-time method and Box-Behnken design response surface methodology was proposed to optimize the important extraction conditions.The experimental results showed that the regression models for the target analytes were all significant(P>0.05).Good linearity with correlation coefficients greater than 0.9981 was obtained under the optimum conditions.The limits of detection(LODs)and limits of quantification(LOQs)were in the range of 2.19–5.35 and 7.30–17.82μg/kg,respectively.The recoveries for spiked samples were between 82.84%and 117.49%with relative standard deviations(RSDs)lower than 9.93%.The present method has the advantages of less solvent consumption,environmental protection and simple operation and thus can be used for the extraction and detection of phenylurea pesticide residues in vegetables.
作者
徐尉力
付壮
王旭
赵悦
王晨兆
马佳骏
王志兵
XU Weili;FU Zhuang;WANG Xu;ZHAO Yue;WANG Chenzhao;MA Jiajun;WANG Zhibing(College of Chemistry and Life Science,Changchun University of Technology,Changchun 130012,China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2020年第4期248-255,共8页
Food Science
基金
国家自然科学基金青年科学基金项目(21401011)
吉林省教育厅“十三五”科学技术项目(JJKH20181014K)
关键词
沉积固化离子液体
均相液液微萃取
苯脲类除草剂
响应面法
蔬菜
高效液相色谱
solidification of sedimentary ionic liquids
homogeneous liquid-liquid microextraction
phenylurea pesticides
response surface analysis
vegetables
high performance liquid chromatography
