Garrido Frenich Antonia, Fernández Moreno José Luis, Martínez Vidal José Luis, Arrebola Liébanas Francisco Javier
Research Group "Analytical Chemistry of Contaminants", Department of Analytical Chemistry, University of Almería, 04071 Almería, Spain.
J Agric Food Chem. 2007 Oct 17;55(21):8346-52. doi: 10.1021/jf071615j. Epub 2007 Sep 18.
A new multiresidue method has been developed and validated for the simultaneous determination of 100 pesticide residues in olive oil. The determination of pesticide residues was carried out in only 19 min by gas chromatography coupled to tandem mass spectrometry using a triple quadrupole mass analyzer. The mass spectrometer was operated in electron ionization and the selection reaction monitoring mode was used, acquiring two or three fragmentation reactions per compound. Two extraction processes were studied, and an evaluation of the stability and sensitivity of the chromatographic system has been performed for the tested extraction procedures. The final proposed methodology was based on a liquid-liquid partition with an n-hexane/acetonitrile mixture followed by a gel permeation chromatography cleanup step. An adequate lineal relation was obtained in the studied concentration range (10-200 microg kg (-1)); the recovery values were in the range 70-110% for the two levels of concentration studied: 12 and 50 microg kg (-1). Precision values, expressed as relative standard deviation, were lower than 18% at the aforementioned spiking levels; detection limits, confirmation limits, and quantitation limits were below or equal to 1.9, 2.6, and 3.6 microg kg (-1), respectively. The developed methodology was applied to the analysis of pesticide residues in real samples of olive oil from the south of Spain.
已开发并验证了一种新的多残留方法，用于同时测定橄榄油中的100种农药残留。使用三重四极杆质量分析仪，通过气相色谱-串联质谱法仅在19分钟内即可完成农药残留的测定。质谱仪采用电子电离模式运行，并使用选择反应监测模式，每种化合物采集两到三个碎片反应。研究了两种萃取方法，并对测试的萃取程序进行了色谱系统稳定性和灵敏度的评估。最终提出的方法基于用正己烷/乙腈混合物进行液-液分配，随后进行凝胶渗透色谱净化步骤。在所研究的浓度范围（10 - 200 μg kg⁻¹）内获得了良好的线性关系；对于所研究的两个浓度水平：12和50 μg kg⁻¹，回收率在70 - 110%范围内。以相对标准偏差表示的精密度值在上述加标水平下低于18%；检测限、确证限和定量限分别低于或等于1.9、2.6和3.6 μg kg⁻¹。所开发的方法应用于西班牙南部橄榄油实际样品中农药残留的分析。
