Botitsi Helen, Economou Anastasios, Tsipi Despina
General Chemical State Laboratory, Pesticide Residues Laboratory, 16 An. Tsoha, 11521 Athens, Greece.
Anal Bioanal Chem. 2007 Nov;389(6):1685-95. doi: 10.1007/s00216-007-1452-3. Epub 2007 Jul 21.
A sensitive multi-residue analytical method, utilizing ethyl acetate extraction and liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS-MS), has been developed and validated for simultaneous determination of 28 pesticides of different chemical classes (polar organophosphates, carbamates, strobilurines, neonicotinoids, amides, pyrimidines, benzimidazoles, imidazoles and triazoles), and their transformation products, in processed fruit and vegetables. Two precursor-product ion transitions were monitored for each pesticide in selected reaction monitoring (SRM) mode. Linearity (r (2) > or = 0.99) was good over the concentration range 0.5 to 100 microg L(-1) for all the pesticides, and instrumental detection limits ranged from 0.1 to 1 microg L(-1). Mean recovery for fruit and vegetables spiked at 0.010 mg kg(-1) ranged from 65 to 94.4%, and relative standard deviations ranged from 9.0 to 20.0%. When the amount spiked was 0.050 mg kg(-1) recoveries ranged from 72.5 to 90% and relative standard deviations were from 6.1 to 19.0%. Method detection limits were from 0.002 to 0.007 mg kg(-1) for the different food matrices studied. The method was used to monitor pesticide residues in a wide variety of fruits and vegetables.
已开发并验证了一种灵敏的多残留分析方法，该方法利用乙酸乙酯萃取和液相色谱-电喷雾电离串联质谱（LC-ESI-MS-MS），用于同时测定加工水果和蔬菜中28种不同化学类别的农药（极性有机磷农药、氨基甲酸酯类、甲氧基丙烯酸酯类、新烟碱类、酰胺类、嘧啶类、苯并咪唑类、咪唑类和三唑类）及其转化产物。在选择反应监测（SRM）模式下，对每种农药监测两个前体-产物离子转换。所有农药在0.5至100 μg L⁻¹浓度范围内线性良好（r²≥0.99），仪器检测限为0.1至1 μg L⁻¹。在0.010 mg kg⁻¹加标水平下，水果和蔬菜的平均回收率为65%至94.4%，相对标准偏差为9.0%至20.0%。当加标量为0.050 mg kg⁻¹时，回收率为72.5%至90%，相对标准偏差为6.1%至19.0%。所研究的不同食品基质的方法检测限为0.002至0.007 mg kg⁻¹。该方法用于监测多种水果和蔬菜中的农药残留。
