Green Analysis: High throughput Analysis of Emerging Pollutants in Plant Sap by Freeze-Thaw-Centrifugal Membrane Filtration Sample Preparation - HPLC-MS/MS Analysis


Emerging and fugitive contaminants (EFCs) released to our biosphere have caused a legacy and continuing threat to human and ecological health, contaminating air, water, and soil. Polluted media are closely linked to food security through plants, especially agricultural crops. However, measuring EFCs in plant tissues remains difficult, and high-throughput screening is a greater challenge. A novel rapid freeze-thaw/centrifugation extraction followed by high performance liquid chromatography - tandem mass spectrometry (HPLC-MS/MS) analysis was developed for high-throughput quantification of 11 EFCs with diverse chemical properties, including estriol, codeine, oxazepam, 2,4-dinitrotoluene, 1,3,5-trinitroperhydro-1,3,5-triazine, bisphenol A, triclosan, caffeine, carbamazepine, lincomycin, and DEET, in three representative crops, corn, tomato, and wheat. The internal aqueous solution, i.e., sap, is liberated via a freeze/thaw cycle, and separated from macromolecules utilizing molecular weight cutoff membrane centrifugal filtration. Detection limits ranged from 0.01 µg L-1 to 2.0 µg L-1. Recoveries of spiked analytes in three species ranged from 83.7% to 109%. Developed methods can rapidly screen EFCs in agriculture crops and can assess pollutant distribution at contaminated sites and gain insight on EFCs transport in plants to assess transmembrane migration in vascular organisms. The findings contribute significantly to environmental research, food security, and human health, as it assesses the first step of potential entry into the food chain, that being transmembrane migration and plant uptake, the primary barrier between polluted waters or soils and our food.



Second Department

Civil, Architectural and Environmental Engineering

Research Center/Lab(s)

Center for Research in Energy and Environment (CREE)


This study was supported by United States National Science Foundation, award number 1606036.

Keywords and Phrases

Agriculture Crops; Emerging And Fugitive Contaminants; Food Safety; Freeze-Thaw-Centrifugation; HPLC-MS/MS Method; Rapid Plant Sample Preparation

International Standard Serial Number (ISSN)

0021-8561; 1520-5118

Document Type

Article - Journal

Document Version


File Type





© 2019 American Chemical Society (ACS), All rights reserved.

Publication Date

01 Oct 2019