摘要
该文建立了一种简单、高效的新型疏水性低共熔溶剂液液微萃取法,用于提取和富集市售包装豆奶中的三嗪类(阿特拉津、去草净)和苯脲类(灭草隆、绿麦隆)除草剂,并结合高效液相色谱对目标分析物进行分离和测定。以六氟异丙醇为氢键供体,四丁基氯化铵为氢键受体,按照不同摩尔比制备了一系列疏水性低共熔溶剂,并对影响萃取效果的实验条件进行了优化,包括低共熔溶剂的种类及用量、氯化钠用量、涡旋时间、pH值和温度。结果表明,在最佳实验条件下,4种目标物在1.00~500.00μg/L范围内具有良好的线性关系(r≥0.9984),检出限和定量下限分别为0.56~0.95μg/L和1.87~3.16μg/L,日内和日间相对标准偏差(RSD)分别为0.28%~2.0%和2.1%~7.5%,加标回收率为86.4%~117%。该方法具有操作简单快速、萃取时间短、试剂用量少和实验成本低等优点,可用于市售包装豆奶中三嗪类和苯脲类除草剂的分析检测。
A novel high performance liquid chromatography(HPLC)with hydrophobic deep eutectic solvent(DES)based liquid-liquid microextraction was developed for the separation and determina⁃tion of triazine(atrazine,terbutryn)and phenylurea(monuron,chlortoluron)herbicides in market packaged soymilk.In this work,a series of new DESs with different molar ratios were synthesized with tetrabutylammonium chloride as hydrogen bond acceptor and hexafluoropropanol as hydrogen bond donor.In addition,the experimental conditions that affect the extraction effect were investigat⁃ed in detail,including type and amount of DESs,amount of NaCl,vortex time,pH value and tem⁃perature.Experimental results showed that,there were good linear relationships for the target analytes in the range of 1.00-500.00μg/L,with correlation coefficients(r)not less than 0.9984.The lim⁃its of detection(LOD,S/N=3)and quantitation(LOQ,S/N=10)were in the range of 0.56-0.95μg/L and 1.87-3.16μg/L,respectively.The relative standard deviations for intra-day and inter-day precision were in the range of 0.28%-2.0%and 2.1%-7.5%,respectively.Recoveries for the target analytes in four spiked samples ranged from 86.4%to 117%,with relative standard deviations of 0.13%-5.7%.With the advantages of simplicity,rapidness,short extraction time,low con⁃sumption and low experimental cost,this method could be used for the analysis and detection of tri⁃azine and phenylurea herbicides in market packaged soy milk.
作者
朱清
龙冰华
陈星航
闫徐
朱红年
冯吉
徐尉力
王志兵
ZHU Qing;LONG Bing-hua;CHEN Xing-hang;YAN Xu;ZHU Hong-nian;FENG Ji;XU Wei-li;WANG Zhi-bing(College of Chemistry and Life Science,Changchun University of Technology,Changchun 130012,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2021年第10期1467-1473,共7页
Journal of Instrumental Analysis
基金
吉林省科技厅项目(20190304011YY)
吉林省教育厅“十四五”科学技术项目(JKH20210762KJ)
国家级大学生创新创业训练计划项目(202010190012)。
关键词
液液微萃取
疏水性低共熔溶剂
三嗪类除草剂
苯脲类除草剂
豆奶
高效液相色谱
liquid-liquid microextraction
deep eutectic solvents
triazine herbicides
phenyl⁃urea herbicides
soy milk
high performance liquid chromatography
