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Analysis of Acid Herbicides in Drinking and Surface Water Using On-line SPE-LC-MS/MS

24 August 2016

Application note AN863 describes the use of ISOLUTE® ENV+ On-line cartridges in a fully automated on-line SPE-LC-MS/MS method for extraction and quantification of 16 acid herbicides in a range of water matrices.


Acidic herbicides cover a broad range of compounds which are widely used in crop protection and general weed control. They tend to be extremely water soluble, and can easily enter surface and ground waters through natural drainage. Acid herbicides are toxic to humans and aquatic organisms, and are therefore monitored to low ng/L levels in potable and ground waters. 

Trace analysis of organics in water traditionally involves large sample volumes, labor intensive procedures and relatively high use of solvents. The on-line SPE approach uses a simple, well established hardware setup, and fully integrates sample preparation into the analytical workflow. Typical sample volumes of 1-10 mL, and lower solvent usage mean sample collection, transport and handling, along with solvent disposal costs, are much reduced. The on-line approach to sample preparation has grown in popularity because of its advantages in improved workflow and reduced sample handling:

  • Little or no sample pre-treatment 
  • Totally automated procedures 
  • High precision and accuracy 
  • Elimination of blow down and reconstitution steps 
  • Reduced solvent use and disposal costs 


The ISOLUTE® ENV+ On-line SPE cartridge provided reproducible pre-concentration of a wide range of acid herbicides in a variety of water matrices. Limits of detection in the low ng/mL range are achievable for all analytes. Reproducibility between batches was seen on the data produced over three separate days. The data was shown to be comparable by using a paired T-test. No carryover was seen in a randomized batch containing blank and spiked samples.


This application vas developed by Russell Gibbs, from a collaborating laboratory (Dwr Cymru Welsh Water) in the UK. The author would like to thank the analysts in the Chemistry Department of DCWW’s Glaslyn Laboratory.

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