摘要
【目的】针对柑橘中常用的农药,采用QuEChERS方法和超高效液相色谱-三重四极杆串联质谱,系统研究了其测定过程中的基质效应。【方法】柑橘样品利用乙酸-乙腈溶液(V∶V=1∶99)提取、GCB净化,采用甲醇-0.1%甲酸水溶液(含1 mmol·L^(-1)乙酸铵)作为流动相,正离子多反应监测(MRM)模式,基质外标法定量,可以有效地减弱基质效应。【结果】10种农药在柑橘中主要是以基质抑制为主,其基质效应范围为-18%~4%,在0.1~100 ng·mL^(-1)内线性关系良好,相关系数(r)大于0.999,检出限为0.08~0.30μg·kg^(-1),回收率为70.5%~102%,相对标准偏差(RSD)为3.32%~5.76%。【结论】该方法快速简便、净化效果好,适合柑橘中常见农药的快速测定。
【Objective】Currently,profenofos,chlorpyrifos,difenoconazole,imidacloprid,prochloraz,acetamiprid,carbendazim,enoylmorpholine,pyraclostrobin,malathion,etc.are commonly used in citrus cultivation.Pesticides with higher detection frequency,such as enoylmorpholine,have no limit requirements and relevant measurement method standards in China’s national standards.On the other hand,the determination methods of pesticides such as prochloraz and pyraclostrobin stipulated in the national standards are gas chromatography and gas chromatography-mass spectrometry,respectively,and the detection sensitivity is not added,and the operation of these methods is complicated.The standard method for the determination of fresh amine requires the high-temperature hydrolysis of prochloraz and liquid-liquid extraction after GC-ECD determination,and pyraclostrobin needs to measure after multiple purifications using C18,Carb and NH2 solid phase extraction columns.The operation steps are complicated,time-consuming and laborious.In the operation process,it is necessary to use toluene with high toxicity,which is harmful to the environment and the operator.With the continuous development of QuEChERS technology combined with ultra-high performance liquid chromatography-triple quadrupole mass spectrometer,it is currently widely used in the determination of a variety of pesticide residues in fruits and vegetables due to its quick and easy operation and high sensitivity.However,for ultrahigh performance liquid chromatography-triple quadrupole mass spectrometer,matrix effect is a common phenomenon in mass spectrometry analysis,especially the complex matrix of citrus,due to the more pigment and essential oil content,its matrix effect is stronger,seriously affecting the accurate quantification of related pesticides in citrus.The matrix effects in the determination of commonly pesticides used in citrus were systematically studied by using the QuEChERS method and ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometr
作者
林涛
陈兴连
刘兴勇
李茂萱
李彦刚
刘宏程
LIN Tao;CHEN Xinglian;LIU Xingyong;LI Maoxuan;LI Yangang;LIU Hongcheng(Institute of Agriculture Quality Standards&Testing Technique,Yunnan Academy of Agricultural Science,Kunming 650205,Yunnan,China;Laboratory of Quality&Safety Risk Assessment for Agro-Products(Kunming),Ministry of Agriculture and Rural Affairs,Kunming 650205,Yunnan,China)
出处
《果树学报》
CAS
CSCD
北大核心
2021年第4期613-622,共10页
Journal of Fruit Science
基金
云南省重大专项计划项目(2018BC005-04)
2019年国家农产品质量安全风险评估项目(GJFP2019012)。
