基于深共晶溶剂的液-液微萃取法结合液相色谱-串联质谱法检测枸杞中的10种农药残留  

Determination of 10 kinds of pesticide residues in wolfberry by liquid-liquid micro-extraction method with deep eutectic solvent combined with liquid chromatography-tandem mass spectrometry

作　　者：陈佳楠 李丹[2] 周一冉 吕峰 吉福墉 连玉晶[1] 王明林[1] 张念英 李雯露 CHEN Jia-Nan;LI Dan;ZHOU Yi-Ran;LV Feng;JI Fu-Yong;LIAN Yu-Jing;WANG Ming-Lin;ZHANG Nian-Ying;LI Wen-Lu(College of Food Science and Engineering,Shandong Agricultural University,Taian 271018,China;Shandong Medicine Technician College,Taian 271016,China;Jining Institute for Food and Drug Control,Jining 272071,China;Rizhao Market Supervision and Testing Center,Rizhao 276800,China;Jining Agricultural Technology Extension Center,Jining 272000,China)

机构地区：[1]山东农业大学食品科学与工程学院,泰安271018 [2]山东医药技师学院,泰安271016 [3]济宁市食品药品检验检测研究院,济宁272071 [4]日照市场监管检验检测中心,日照276800 [5]济宁市农业技术推广中心,济宁272000

出　　处：《食品安全质量检测学报》2021年第12期4793-4800,共8页Journal of Food Safety and Quality

基　　金：“十三五”国家重点研发计划项目(2018YFC1602302);山东省重点研发计划项目(2019JZZY020903)。

摘　　要：目的建立基于深共晶溶剂的液-液微萃取结合液相色谱-串联质谱法检测枸杞中10种农药多残留的分析方法。方法通过氢键供体和受体的组成及合成比例、深共晶溶剂的密度、粘度和傅里叶红外光谱分析对深共晶溶剂进行优化表征。在50℃恒温条件下,分别以深共晶溶剂为萃取剂,四氢呋喃为乳化剂,通过涡旋和超声进行提取。离心后实现两相分离,下层深共晶溶剂相用甲醇-水(50:50, V:V)稀释上样。结果目标物在0.01~50.0μg/kg范围内线性关系良好,线性相关系数均大于0.9997,方法的检出限和定量限分别为0.0088~0.5952μg/kg和0.0294~1.9814μg/kg。在3个加标水平(0.2、2.0、20.0μg/kg)下, 10种农药的回收率分别为79.8%~99.4%, 82.3%~101.8%和88.5%~102.4%,相对标准偏差均小于15.0%,符合多农药残留检测要求。结论该方法操作简单、准确度高,适用于枸杞中农药残留等污染物的检测。Objective To establish a method for determination of 10 kinds of pesticide residues in wolfberry by liquid-liquid micro-extraction method based on deep eutectic solvents combined with liquid chromatography-tandem mass spectrometry. Methods The deep eutectic solvents were optimized and characterized by the composition and synthesis ratio of hydrogen bond donors and acceptors, the density and viscosity of the deep eutectic solvents, and fourier transform infrared spectroscopy. At a constant temperature of 50 ℃, the deep eutectic solvent was used as the extractant and tetrahydrofuran was used as the emulsifier. The extraction was carried out by vortex and ultrasound. The two-phase separation was realized after centrifugation. The lower deep eutectic solvent phase was diluted with methanol water(50:50, V:V). Results The linear relationship of the targets were good in the range of 0.01-50.0 μg/kg, and the linear correlation coefficients were greater than 0.9997. The limits of detection and limits of quantitative of the method were 0.0088-0.5952 μg/kg and 0.0294-1.9814 μg/kg, respectively. The recoveries of 10 pesticides at 3 fortification levels(0.2, 2.0, 20.0 μg/kg) were 79.8%-99.4%, 82.3%-101.8% and 88.5%-102.4%, respectively. The relative standard deviations were all less than 15.0%, which met the requirements of pesticide residue detection. Conclusion This method is simple and accurate, and is suitable for the determination of pesticide residues and other pollutants in wolfberry.

关 键 词：深共晶溶剂 枸杞 农药残留 液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] TS207.53[理学—化学]