Fully Automated QuEChERS Extraction and Clean-up of Organophosphate Pesticides in Orange Juice

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Abstract

A fully automated QuEChERS extraction and extract clean-up method for GC-MS and LC-MS analysis is presented by using an industry standard robotic x,y,z-sampling system. The application describes the analysis of organophosphate pesticides from homogeneous liquid samples, as an example orange juice was used. The automated workflow includes the extraction with acetonitrile, salting out and using a µSPE cartridge for matrix clean-up prior to injection into a GC-MS/MS system. The method validation techniques such as pre-spike and post-spike were fully integrated into the automated workflow as well. Calibration linearities of the applied organophosphate pesticides in orange juice matrix range from 1 to 100 ng/mL with a precision achieved better than 0.995 for all compounds. By spiking 10 ng/mL of pesticides into the orange juice samples, recoveries were obtained in the of range 70% – 115%, while the precision from pre-spike (n=7) and post-spikes (n=6) under the same concentration was less than 10% RSD. The calculated method detection limits (MDLs) of the monitored pesticides were in the range of 1.8 ng/mL to 4.1 ng/mL which are well below the regulated maximum residue limits (MRLs) of 10 ng/g for these pesticides.

Publisher

Uniscience Publishers LLC

Reference11 articles.

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2. QuEChERS, https://www.quechers.com/index.php (as of Jan 11, 2021)

3. Lehotay, S. J., Michlig, N., & Lightfield, A. R. (2020). Assessment of Test Portion Sizes after Sample Comminution with Liquid Nitrogen in an Improved High-Throughput Method for Analysis of Pesticide Residues in Fruits and Vegetables. J. Agric. Food Chem. 68(5), 1468-1479. https://doi.org/10.1021/acs.jafc.9b07685

4. Directorate-General for Health and Food Safety (2017). SANTE 11312/2021 Guidance Document on Analytical Quality Control and Validation Procedures for Pesticide Residues Analysis in Food and Feed. European Commission Health & Consumer Protection Directorate General.

5. Ekroth, S. (2017). The SweEt Method: An Efficient Alternative to Analyze Pesticide Residues in Food. National Food Administration (NFA) Sweden, presented at the LAPRW Conference, San Jose, Costa Rica, 2017.

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