Tippannanavar Madhu, Banerjee Tirthankar, Shekhar Sumit, Sahu Sudama Ram, Singh Bijendra, Narayanan Neethu, Rudra Shalini Gaur, Chakrabarti Bidisha, Gupta Suman, Singh Anupama
Division of Agricultural Chemicals, New Delhi, India.
The Graduate School, New Delhi, India.
Front Chem. 2023 Nov 21;11:1283895. doi: 10.3389/fchem.2023.1283895. eCollection 2023.
A robust method was developed using LC-ESI-MS/MS-based identification and quantification of 103 fortified pesticides in a mango fruit drink. Variations in QuEChERS extraction (without buffer, citrate, and/or acetate buffered) coupled with dispersive clean-up combinations were evaluated. Results showed 5 mL dilution and citrate buffered QuEChERS extraction with anhydrous (anhy) MgSO clean-up gave acceptable recovery for 100 pesticides @ 1 μg mL fortification. The method was validated as per SANTE guidelines (SANTE/11813/2021). 95, 91, and 77 pesticides were satisfactorily recovered at 0.1, 0.05, and 0.01 μg mL fortification with HorRat values ranging from 0.2-0.8 for the majority. The method showed matrix enhancement for 77 pesticides with a global uncertainty of 4.72%-23.89%. The reliability of the method was confirmed by real sample analysis of different brands of mango drinks available in the market. The greenness assessment by GAPI (Green Analytical Procedure Index) indicated the method was much greener than other contemporary methods.
开发了一种基于液相色谱-电喷雾串联质谱法（LC-ESI-MS/MS）对芒果果汁饮料中103种加标农药进行鉴定和定量的稳健方法。评估了QuEChERS萃取法（无缓冲液、柠檬酸盐和/或醋酸盐缓冲液）与分散净化组合的变化情况。结果表明，5 mL稀释液和用无水硫酸镁净化的柠檬酸盐缓冲QuEChERS萃取法，对于100种加标量为1 μg/mL的农药，回收率良好。该方法按照SANTE指南（SANTE/11813/2021）进行了验证。在加标量为0.1、0.05和0.01 μg/mL时，分别有95、91和77种农药的回收率令人满意，大多数农药的HorRat值在0.2至0.8之间。该方法对77种农药显示出基质增强效应，总体不确定度为4.72%-23.89%。通过对市场上不同品牌芒果饮料的实际样品分析，证实了该方法的可靠性。通过绿色分析程序指数（GAPI）进行的绿色度评估表明，该方法比其他当代方法更环保。
