首页> 外文会议>IMEKOFOODS Conference >LARGE SCALE MULTI-RESIDUE METHODSBY GAS AND LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY FOR THE DETERMINATION OF PESTICIDE RESIDUES IN FOOD MATRICES
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LARGE SCALE MULTI-RESIDUE METHODSBY GAS AND LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY FOR THE DETERMINATION OF PESTICIDE RESIDUES IN FOOD MATRICES

机译:气体和液相色谱 - 质谱法测定食品基质中农药残留量的大规模多残基方法

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Nowadays, more than 1600 pesticides belonging to more than 100 chemical classes are in use worldwide for food production. In the EU, Regulation (EC) 396/2005 sets maximum pesticide residue limits in food (MRLs), the majority of which ranges over the concentration range 0.01-1 mg/kg. Large scale multi-residue methods based on general extraction procedures in combination with hyphenated instrumental analysis techniques such as gas and liquid chromatography with mass spectrometry are currently used in analytical laboratories working in the field of Pesticide Residues Analysis. In our laboratory, a multi-residue method based on QuEChERS method in combination with LC-MS/MS and GC-MS/MS techniques has been developed for the detection and quantification of pesticide residues, parent compounds and their metabolites, in various food matrices, fulfilling the performance criteria established in the European Union guidelines (SANTE Doc. No 11945/2015). A LC-MS/MS method using QqQ-MS technology in the SRM acquisition mode has been developed for the analysis of more than 250 compounds. Additionally, a GC-MS/MS method using Ion-Trap MSn technology has been applied for the determination of more than 80 GC-amenable compounds. More than 2000 pesticide/food commodity combinations have been validated using the LC- and GC-MS/MS methods, achieving recoveries in the range 70-120% with reproducibility values in terms of relative standard deviations less than 20%; limits of quantification of 0.01mg/Kg were established in most of the cases. Both methods have been successfully applied for the monitoring of multiclass pesticide residues in food samples in the frame of National and EU - Multi Annual Coordinated Control Programs.
机译:如今,属于100多种化学课程的超过1600种农药在全球范围内用于粮食生产。在欧盟,调节(EC)396/2005在食物(MRLS)中置于最大农药残留物限制,其中大部分范围范围为0.01-1mg / kg。基于一般提取程序的大规模多残基方法与连字型仪器分析技术相结合,例如气体和液相色谱,目前用于农药残留分析领域的分析实验室。在我们的实验室中,已经开发了基于QueChers方法的多核方法与LC-MS / MS和GC-MS / MS技术组合用于检测和定量各种食物基质中的农药残留物,母体化合物及其代谢物的检测和定量,履行欧洲联盟指南中建立的绩效标准(Sante Doc。没有11945/2015)。已经开发了在SRM采集模式下使用QQQ-MS技术的LC-MS / MS方法,用于分析超过250种化合物。另外,已经施加了使用离子阱MSN技术的GC-MS / MS方法用于测定超过80种GC-甜味的化合物。使用LC和GC-MS / MS方法验证了2000多种农药/食品组合,在相对标准偏差方面,在70-120%的范围内实现了70-120%的回收率;在大多数情况下建立了0.01mg / kg的量化限制。两种方法已成功应用于国家和欧盟多年协调控制方案框架中食品样本中的多种素农药残留的方法。

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