Ballesteros E, García Sánchez A, Ramos Martos N
Department of Physical and Analytical Chemistry, EPS of Linares, University of Jaén, Alfonso X, Linares, Spain.
J Chromatogr A. 2006 Apr 7;1111(1):89-96. doi: 10.1016/j.chroma.2006.01.101. Epub 2006 Feb 9.
A multiresidue method for determining major pesticides and polycyclic aromatic hydrocarbons (PAHs) in olive oils in a single injection by use of gas chromatography/tandem mass spectrometry (GC-MS/MS) is proposed. Samples are previously extracted with an acetonitrile/n-hexane mixture and cleaned up by gel permeation chromatography. Electron ionization and chemical ionization allow pesticides and PAHs to be determined in a single analysis. The precision obtained was quite satisfactory (relative standard deviations ranged from 3 to 7.8%), and so were recoveries (84-110%). The linear relation was observed from 1 to 500 microg/kg for pesticides and 0.3 to 200 microg/kg for PAHs; also, the determination coefficient, R(2), was better than 0.995 in all instances. The proposed method was applied to the routine analysis of PAH and pesticide residues in virgin and refined olive oil and olive-pomace oil samples.
提出了一种利用气相色谱/串联质谱（GC-MS/MS）单次进样测定橄榄油中主要农药和多环芳烃（PAHs）的多残留方法。样品先用乙腈/正己烷混合物萃取，然后通过凝胶渗透色谱法净化。电子电离和化学电离使得农药和多环芳烃能够在一次分析中同时测定。获得的精密度相当令人满意（相对标准偏差范围为3%至7.8%），回收率也是如此（84%至110%）。农药的线性关系在1至500微克/千克范围内观察到，多环芳烃的线性关系在0.3至200微克/千克范围内观察到；此外，在所有情况下，测定系数R²均优于0.995。该方法应用于初榨橄榄油、精炼橄榄油和橄榄果渣油样品中多环芳烃和农药残留的常规分析。
