Páleníková Agneša, Martínez-Domínguez Gerardo, Arrebola Francisco Javier, Romero-González Roberto, Hrouzková Svetlana, Garrido Frenich Antonia
a Resarch Group "Analytical Chemistry of Contaminants", Department of Chemistry and Physics, Research Centre for Agricultural and Food Biotechnology (BITAL) , University of Almería, Agrifood Campus of International Excellence , Almería , Spain.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2015;32(6):849-56. doi: 10.1080/19440049.2015.1028481. Epub 2015 Apr 14.
The purpose of this study was to evaluate the presence of pesticide residues and transformation products in dietary supplement products. Thirty-two samples were analysed to determine 177 pesticides by gas chromatography-tandem mass spectrometry (GC-MS/MS) and 333 pesticides by liquid chromatography-high-resolution mass spectrometry (LC-HRMS). Pesticides were extracted from different kinds of dietary supplements by the use of a modified QuEChERS extraction method. Six samples contained pesticide residues at concentration up to 92.7 µg kg(-1), but only butralin exceeded the maximum residue limits set for raw material. In addition to target compounds, LC-HRMS enables the simultaneous detection of non-target pesticides. In this case, transformation products of pesticides were detected in the analysed samples using HRMS analyser (Exactive-Orbitrap). These compounds were not included in the original method, and they were monitored as post-target compounds, knowing their molecular formula and exact mass. Mass accuracy was always < 2 ppm, corresponding to a maximum mass error. The positive findings endorse the idea that a deeper and continuous investigation of pesticide residues and transformation products in dietary supplement products is necessary in order to guaranty consumer's safety.
本研究的目的是评估膳食补充剂产品中农药残留和转化产物的存在情况。通过气相色谱-串联质谱法（GC-MS/MS）分析了32个样品中的177种农药，通过液相色谱-高分辨质谱法（LC-HRMS）分析了333种农药。采用改良的QuEChERS萃取方法从不同种类的膳食补充剂中提取农药。6个样品含有浓度高达92.7 μg kg⁻¹的农药残留，但只有仲丁灵超过了为原料设定的最大残留限量。除目标化合物外，LC-HRMS还能同时检测非目标农药。在这种情况下，使用高分辨质谱仪（Exactive-Orbitrap）在分析样品中检测到了农药的转化产物。这些化合物未包含在原始方法中，鉴于其分子式和精确质量，将它们作为目标后化合物进行监测。质量准确度始终<2 ppm，对应最大质量误差。这些阳性结果支持了这样一种观点，即为了保证消费者安全，有必要对膳食补充剂产品中的农药残留和转化产物进行更深入、持续的调查。
