固相萃取-液相色谱-飞行时间质谱法快速筛查与确证谷物和果蔬中25种杀菌剂残留

发布时间：2018-06-15 13:46

  本文选题：杀菌剂 + 固相萃取　； 参考：《分析化学》2017年08期

【摘要】：利用固相萃取-液相色谱-飞行时间质谱(SPE-LC-Q-TOF/MS)技术建立了谷物、蔬菜和水果中25种杀菌剂农药残留的快速筛查和确证检测方法。样品经1%(V/V)乙酸-乙腈溶液提取,经Crabon/NH_2柱净化,乙腈-甲苯(3∶1,V/V)洗脱,C_(18)色谱柱分离,乙腈和0.1%甲酸溶液(含5 mmol/L乙酸铵)梯度洗脱,采用LC-Q-TOF/MS检测,外标法定量。建立了25种杀菌剂的一级精确质量数据库和二级谱图库,通过化合物的精确质量数、保留时间、同位素峰分布、同位素比例等信息对检测结果进行自动检索,在无对照标准品的情况下实现了25种农药的定性鉴定。结果表明,25种杀菌剂在0.02~200μg/L范围内线性关系良好,相关系数R2≥0.9950,加标回收率在71.8%~114.0%之间,相对标准偏差(RSD)为0.1%~21.3%(n=3)。25种杀菌剂检出限为0.01~5.00μg/kg,定量限为0.02~20.00μg/kg。本方法简便、快速、可靠,可用于谷物、蔬菜、水果中25种杀菌剂的快速筛查。
[Abstract]:The SPE-LC-Q-TOF / MS technique of SPE-LC-Q-TOF / MS was used to establish a rapid screening and identification method for the pesticide residues of 25 fungicides in cereals, vegetables and fruits. The samples were extracted by acetonitrile solution of V / V, purified by Crabon / NH _ 2 column, eluted by acetonitrile-toluene 3: 1 V / V) column, separated by acetonitrile and 0.1% formic acid solution (containing 5 mmol / L ammonium acetate) by gradient elution, detected by LC-Q-TOF / MS and quantified by external standard method. The first order accurate mass database and the second order spectrum map database of 25 kinds of fungicides were established. The detection results were automatically retrieved by the information of accurate mass number, retention time, isotope peak distribution and isotope ratio of compounds. The qualitative identification of 25 pesticides was carried out without the control standard. The results showed that the linear range of 25 fungicides was within the range of 0.02 ~ 200 渭 g / L, the correlation coefficient R ~ 2 鈮，

本文编号：2022200