采用液相色谱-串联质谱法监测食用油和坚果中的极性农药和污染物。
Monitoring of polar pesticides and contaminants in edible oils and nuts by liquid chromatography-tandem mass spectrometry.
机构信息
Department of Chemistry and Physics, Analytical Chemistry Area, University of Almería, Research Centre for Mediterranean Intensive Agrosystems and Agri-Food Biotechnology (CIAIMBITAL), Agrifood Campus of International Excellence ceiA3, Carretera de Sacramento s/n, E-04120 Almería, Spain.
Department of Chemistry and Physics, Analytical Chemistry Area, University of Almería, Research Centre for Mediterranean Intensive Agrosystems and Agri-Food Biotechnology (CIAIMBITAL), Agrifood Campus of International Excellence ceiA3, Carretera de Sacramento s/n, E-04120 Almería, Spain.
出版信息
Food Chem. 2021 May 1;343:128495. doi: 10.1016/j.foodchem.2020.128495. Epub 2020 Nov 1.
A single method was developed for the determination of polar pesticides (fosetyl-Al and its metabolite, phosphonic acid, and ethephon) and environmental contaminants (chlorate and perchlorate) in edible oils and nuts. Two extraction methods based on QuPPe-PO approach (Quick Polar Pesticides Method for products of Plant Origin) were optimized. In oils, a single extraction using water acidified with formic acid (1%) was performed, while in nuts, the clean-up step was modified. C18 was used as sorbent and an extra cleaning step with n-hexane was added. The extracts were analysed by liquid chromatography coupled to a triple quadrupole mass analyser (LC-QqQ-MS/MS). The method was validated and the limit of quantification was 0.01 mg kg for all analyte-matrix combination. Recoveries from 70 to 120%, and intra and inter-day precision values ≤20% were obtained. Forty samples of edible oils and nuts were analysed, detecting phosphonic acid in nuts at concentrations up to 4.6 mg kg.
开发了一种单一方法，用于测定食用油和坚果中的极性农药（福赛膦及其代谢物膦酸和乙烯利）和环境污染物（氯酸盐和高氯酸盐）。优化了两种基于 QuPPe-PO 方法（植物源产品的快速极性农药方法）的提取方法。在油中，使用酸化至 1%甲酸的水进行单一提取，而在坚果中，修改了净化步骤。C18 用作吸附剂，并添加了用正己烷进行的额外清洁步骤。提取物通过液相色谱-串联三重四极杆质谱（LC-QqQ-MS/MS）进行分析。该方法经过验证，所有分析物-基质组合的定量限为 0.01 mg kg。回收率为 70%至 120%，日内和日间精密度值≤20%。分析了 40 个食用油和坚果样本，在坚果中检测到最高浓度达 4.6 mg kg 的膦酸。
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