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Synthesis and application of molecularly imprinted silica for the selective extraction of some polar organophosphorus pesticides from almond oil
Analytica Chimica Acta ( IF 6.2 ) Pub Date : 2018-03-19
Sara Boulanouar, Audrey Combès, Sakina Mezzache, Valérie Pichon

The aim of this work was to prepare and evaluate molecularly imprinted polymers obtained by a sol-gel approach for the selective solid-phase extraction (SPE) of organophosphorus pesticides (OPs) from almond oil. The performances of molecularly imprinted silicas (MISs), prepared using different conditions of synthesis, were studied by applying different extraction procedures in order to determine the ability of the MISs to selectively extract ten target OPs. For this, the retention of OPs on MISs in pure media was compared with the retention on a non-imprinted silicas (NISs), used as control sorbent, to prove the presence of specific cavities. The most promising MIS allowed the selective extraction of the 3 most polar OPs among the 10 studied. The capacity was studied and the repeatability of the extraction recovery yield was demonstrated both in pure and real media. This MIS was able to selectively extract fenthion sulfoxide and dimethoate contained in almond oil extract after applying the optimized extraction procedure with recovery yields between 100 and 114%. The estimated limit of quantification (LOQ, S/N=10), thanks to LC/MS analysis in MRM mode, between 1.2 and 4.6 μg/kg for those OPs in the almond fruits, was more than 10 times lower than the Maximum Residue Levels (MRLs) established by the European Commission. This MIS therefore shows a high potential for the analysis of those two polar OPs at trace levels from almond oils.



中文翻译:

分子印迹二氧化硅的合成及在杏仁油中选择性萃取某些极性有机磷农药的应用

这项工作的目的是制备和评估通过溶胶-凝胶法从杏仁油中选择性固相萃取有机磷农药(OPs)的分子印迹聚合物。通过应用不同的提取程序,研究了使用不同的合成条件制备的分子印迹二氧化硅(MIS)的性能,以确定MIS选择性提取十种目标OP的能力。为此,将OP在纯介质中在MIS上的保留与在非压印二氧化硅(NIS)(用作对照吸附剂)上的保留进行了比较,以证明存在特定的孔洞。最有前途的MIS可在10个研究对象中选择性提取3个极性最大的OP。研究了容量,并在纯介质和真实介质中均论证了提取回收率的可重复性。在应用优化的提取程序后,该MIS能够选择性地提取杏仁油提取物中所含的亚硫磷和乐果的亚硫氰酸盐,回收率在100%至114%之间。由于在MRM模式下进行了LC / MS分析,估计的定量限(LOQ,S / N = 10)在杏仁果实中的OPs在1.2至4.6μg/ kg之间,比最大残留量低10倍以上欧盟委员会制定的级别(MRL)。因此,该MIS在分析杏仁油中痕量水平的这两种极性OP时显示出很高的潜力。在应用优化的提取程序后,该MIS能够选择性地提取杏仁油提取物中所含的硫磷和二甲硫磷,回收率在100%至114%之间。由于在MRM模式下进行了LC / MS分析,估计的定量限(LOQ,S / N = 10)在杏仁果实中的OPs在1.2至4.6μg/ kg之间,比最大残留量低10倍以上欧盟委员会制定的级别(MRL)。因此,该MIS在分析杏仁油中痕量水平的这两种极性OP时显示出很高的潜力。在应用优化的提取程序后,该MIS能够选择性地提取杏仁油提取物中所含的硫磷和二甲硫磷,回收率在100%至114%之间。由于在MRM模式下进行了LC / MS分析,估计的定量限(LOQ,S / N = 10)在杏仁果实中的OPs在1.2至4.6μg/ kg之间,比最大残留量低10倍以上欧盟委员会制定的级别(MRL)。因此,该MIS在分析杏仁油中痕量水平的这两种极性OP时显示出很高的潜力。比欧盟委员会规定的最大残留量(MRL)低10倍以上。因此,该MIS在分析杏仁油中痕量水平的这两种极性OP时显示出很高的潜力。比欧盟委员会规定的最大残留量(MRL)低10倍以上。因此,该MIS在分析杏仁油中痕量水平的这两种极性OP时显示出很高的潜力。

更新日期:2018-03-20
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