Amendola Graziella, Pelosi Patrizia, Attard Barbini Danilo
a National Institute of Health , Department of Environment and Primary Prevention , Rome , Italy.
J Environ Sci Health B. 2015;50(2):109-20. doi: 10.1080/03601234.2015.975607.
A simple, fast and multiresidue method for the determination of pesticide residues in baby foods of animal origin has been developed in order to check the compliance with the Maximum Residue Levels (MRLs) set at a general value of 0.01 mg/kg by Commission Directive 2006/125/EC for infant foods. The main classes of organochlorine, organophosphorus and pyrethroid compounds have been considered, which are mainly fat soluble pesticides. The analytical procedure consists in the extraction of baby food samples by acetonitrile (ACN) followed by a clean up using C18 solid-phase extraction column eluted with ACN. The compounds were determined by gas chromatography-triple quadrupole mass spectrometry equipped with a Programmed Temperature Vaporizer (PTV) injection and a backflush system. In order to compensate for matrix effects PTV and matrix matched standard calibrations have been used. The method has been fully validated for 57 pesticides according to the Document SANCO/12571/2013. Accuracy and precision (repeatability) have been studied by recoveries at two spiking levels, the Limit of Quantitation (LOQ) (0.003-0.008 mg/kg) and 10 time greater (0.03-0.08 mg/kg), and the results were in the acceptable range of 70-120% with Relative Standards Deviations (RSD) ≤20%. Selectivity, linearity, LOQ and uncertainty of measurement were also determined for all the compounds. The method has been also applied for the analysis of 18 baby food animal origin samples, bought form the local market in Rome (Italy), and no pesticide in the scope of the method has been found above the MRL or the LOQ.
为检查婴儿动物源性食品中的农药残留是否符合欧盟委员会指令2006/125/EC为婴儿食品设定的0.01毫克/千克的最大残留限量（MRLs），已开发出一种简单、快速且多残留的方法来测定婴儿动物源性食品中的农药残留。该方法考虑了主要的有机氯、有机磷和拟除虫菊酯类化合物，这些主要是脂溶性农药。分析程序包括用乙腈（ACN）提取婴儿食品样品，然后使用C18固相萃取柱进行净化，并用ACN洗脱。通过配备程序升温汽化器（PTV）进样和反吹系统的气相色谱 - 三重四极杆质谱法测定这些化合物。为补偿基质效应，使用了PTV和基质匹配标准校准。根据文件SANCO/12571/2013，该方法已针对57种农药进行了全面验证。通过在两个加标水平下的回收率研究了准确度和精密度（重复性），定量限（LOQ）为0.003 - 0.008毫克/千克和其10倍浓度（0.03 - 0.08毫克/千克），结果在70 - 120%的可接受范围内，相对标准偏差（RSD）≤20%。还测定了所有化合物的选择性、线性、LOQ和测量不确定度。该方法还应用于分析从意大利罗马当地市场购买的18份婴儿动物源性食品样品，未发现该方法范围内的农药残留超过MRL或LOQ。
