Fernández Remedios, Garrido Frenich Antonia, Martínez Vidal José Luis, Romero González Roberto, Hernández Torres María Elena
Laboratory of Pesticide Residues LAB, Calablanca Bajo, 04009 Almería, Spain.
Anal Sci. 2009 Apr;25(4):535-40. doi: 10.2116/analsci.25.535.
A rapid method has been developed for monitoring five multiclass pesticides commonly used in citrus fruits. The determination is performed by ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS), after extraction with a mixture of ethyl acetate and sodium sulfate. The method has been validated for orange matrix. Mean recoveries obtained were between 74-110% with a repeatability precision of < 7%, intermediate precision of < 10% and reproducibility precision of < 17%. Linearity over the range 0.010-0.150 mg/kg was demonstrated (r(2) > or = 0.99) with limits of quantification (LOQs) of < or = 0.01 mg/kg. Also, an analytical study focused on the stability of pesticide residues in orange extracts under storage was performed. The method has been applied to the analysis of 365 samples from the agricultural area of the Valencian Community (Spain). Of 103 samples that contained pesticide residues, only abamectin in 2 samples and carbendazim in 5 samples slightly exceeded the European maximum residue limits (MRLs).
已开发出一种快速方法，用于监测柑橘类水果中常用的五种多类农药。在用乙酸乙酯和硫酸钠的混合物萃取后，通过超高效液相色谱-串联质谱法（UPLC-MS/MS）进行测定。该方法已在橙子基质中得到验证。获得的平均回收率在74%-110%之间，重复性精密度<7%，中间精密度<10%，再现性精密度<17%。在0.010-0.150 mg/kg范围内证明了线性关系（r(2)≥0.99），定量限（LOQs）≤0.01 mg/kg。此外，还进行了一项分析研究，重点关注橙子提取物中农药残留的储存稳定性。该方法已应用于对来自西班牙巴伦西亚自治区农业区的365个样品的分析。在103个含有农药残留的样品中，只有2个样品中的阿维菌素和5个样品中的多菌灵略微超过了欧洲最大残留限量（MRLs）。
