Rapid determination of acid herbicides in soil by liquid chromatography with tandem mass spectrometric detection based on dispersive solid phase extraction

Abstract

This study determined twenty six the highly sensitive phenoxy, pyridines, aliphatic and aromatic acid compounds in soil with a liquid chromatography tandem mass spectrometry. The samples were prepared by modified quick, easy, cheap, effective, rugged and safe (QuEChERS) analytical procedure in solid samples. Herbicides extraction effectiveness was evaluated at three different spiking levels (0.01, 0.1 and 1.0mgkg−1). Fourteen different dispersive solid-phase extraction (d-SPE) sorbents in clean-up step were tested. The QuEChERS protocol with acidic alumina provided the highest number of pesticides with recoveries in the 70–120% range. The soil matrix effect was evaluated and for the majority of compounds were not significant, showing suppression or enhancement (±81–123%). The precision calculated as relative standard deviation (RSD) was below 22%. The linear relation was observed in the range 0.01–2.0mgkg−1 and the correlation coefficient R>0.999. The expanded measurement uncertainty was estimated as being on average, and was between 9% and 33%. The validated method was employed in the analysis of 309 real soil samples.