采用 LC-MS/MS 法同时测定石榴全果和石榴籽中的农药残留。
Simultaneous determination of pesticide residues in pomegranate whole fruit and arils using LC-MS/MS.
机构信息
All India Network Project on Pesticide Residue, Pesticide Residue and Food Quality Analysis Laboratory, University of Agricultural Sciences, Raichur 584 104, Karnataka, India.
All India Network Project on Pesticide Residue, Pesticide Residue and Food Quality Analysis Laboratory, University of Agricultural Sciences, Raichur 584 104, Karnataka, India.
出版信息
Food Chem. 2022 Sep 1;387:132865. doi: 10.1016/j.foodchem.2022.132865. Epub 2022 Mar 31.
An analytical method in pomegranate whole fruits and arils was developed in LC-MS/MS and validated as per SANTE/12682/2019. Samples were extracted following acetonitrile-based modified QuEChERS protocol. The method was linear and the coefficient of determination ranged between 0.998 and 0.999. Through this method, all the pesticides were detected and quantified at 10 µg kg. The accuracy test at 10, 50, and 100 µg kg spiking level recorded recovery between 70 and 120% and RSD less than 15% in both matrices. No significant matrix effect was observed for most pesticides. Intra (RSDr) and inter-day (RSDwr) precision estimated at 50 µg kg found acceptable RSD in both matrices. Measurement uncertainty at 50 µg kg was in the range of 4.02 to 16.12 µg kg. Quantifying pesticides in pomegranate whole fruits, peel, and arils using the proposed method is highly suitable and reproducible for 74 pesticides in a short run time of 25.00 min.
建立了 LC-MS/MS 分析方法，并按照 SANTE/12682/2019 进行了验证，用于石榴全果和石榴籽中 74 种农药的检测。样品采用基于乙腈的改良 QuEChERS 前处理方法提取。方法线性良好，相关系数在 0.998 至 0.999 之间。通过该方法可在 10μg/kg 水平下同时检测和定量所有农药。在 10、50 和 100μg/kg 加标水平下的准确度试验，在两种基质中回收率均在 70%至 120%之间，RSD 均小于 15%。大多数农药在基质中均未观察到明显的基质效应。在 50μg/kg 水平下，日内（RSDr）和日间（RSDwr）精密度在两种基质中均具有可接受的 RSD。在 50μg/kg 水平下测量不确定度在 4.02 至 16.12μg/kg 之间。该方法在 25.00min 的短运行时间内，适用于石榴全果、果皮和石榴籽中 74 种农药的快速检测，重现性好。
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