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基于 QuEChERS 方法的测定茶类营养保健品中农药残留的液相色谱-串联三重四级杆质谱法

Application of QuEChERS based method for the determination of pesticides in nutraceutical products (Camellia sinensis) by liquid chromatography coupled to triple quadrupole tandem mass spectrometry.

机构信息

Research 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, CeiA3, E-04120 Almería, Spain.

Research 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, CeiA3, E-04120 Almería, Spain.

出版信息

Food Chem. 2015 Jun 15;177:182-90. doi: 10.1016/j.foodchem.2015.01.032. Epub 2015 Jan 9.

DOI:10.1016/j.foodchem.2015.01.032
PMID:25660875
Abstract

A QuEChERS (quick, easy, cheap, effective, rugged, and safe) based method has been evaluated and validated for the determination and quantification of approximately 100 LC-amenable pesticides in nutraceutical products obtained from green tea (Camellia sinensis). Extraction was performed with acidified acetonitrile (acetic acid 1% (v/v)), and additional clean-up steps were not necessary. Pesticides determination was achieved using ultra high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry (UHPLC-QqQ-MS/MS). Total running time was 11 min. Pesticides were quantified using matrix-matched calibration. Recoveries ranged from 70% to 117% and relative standard deviation (RSD) was lower than 20% at concentration levels of 25, 50 and 100 μg/kg for intra-day precision and equal or lower than 25% for inter-day precision. Limits of quantification (LOQ) were equal or lower than 25 μg/kg. The validated method was applied to commercial nutraceutical products, detecting acetamiprid (56 μg/kg) and carbendazim (13 μg/kg) in two samples.

摘要

建立了一种基于 QuEChERS 的方法,用于测定和定量分析来源于绿茶(Camellia sinensis)的营养保健品中约 100 种可液相色谱分析的农药。采用酸化乙腈(乙酸 1%(v/v))提取,无需进一步净化步骤。采用超高效液相色谱-串联三重四极杆质谱(UHPLC-QqQ-MS/MS)进行农药检测。总运行时间为 11 分钟。采用基质匹配校准法定量。在 25、50 和 100μg/kg 浓度水平下,日内精密度的回收率在 70%至 117%之间,相对标准偏差(RSD)低于 20%;日间精密度的 RSD 等于或低于 25%。定量限(LOQ)等于或低于 25μg/kg。该方法已应用于商业营养保健品,在两个样品中检测到了乙酰甲胺磷(56μg/kg)和多菌灵(13μg/kg)。

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