Determination of residues of sulfonylurea herbicides in soil by using microwave-assisted extraction and high performance liquid chromatographic method

Nada L. Grahovac, Zorica S. Stojanović, Snežana Ž. Kravić, Dejan Z. Orčić, Zvonimir J Suturović, Ankica Đ. Kondić-Špika, Jovica R. Vasin, Dragana B. Šunjka, Snežana P. Jakšić, Miloš M. Rajković, Nenad M. Grahovac


A modified method for the analysis of nicosulfuron, rimsulfuron and prosulfuron was developed and validated by using microwave-assisted extraction (MAE) and ultra-perform­ance liquid chromatography with diode array detection in the ultraviolet region (HPLC-UV-DAD). The most important experimental parameters of extraction procedure and HPLC-UV-DAD technique were optimised in respect to those sulfonylurea herbicides. High rec­overies of the microwave-assisted extraction were obtained by using a dichloromethaneacetonitrile mixture (2:1 volume ratio) acidified with acetic acid (0.8 vol.%) with the addit­ion of urea. The mean recoveries at three spiking levels ranged from 97.47 to 98.76% for nicosulfuron, 97.88 to 99.17% for rimsulfuron and from 97.91 to 99.83% for prosulfuron. The limits of detection of nicosulfuron, rimsulfuron and prosulfuron were 0.95, 0.91 and 0.89 µg kg–1, respectively. The accuracy of the developed method was confirmed by HPLC coupled with tandem mass spectrometry parallel analyses. The developed method was used to investigate the dissipation dynamics of sulfonylurea herbicides in the real field trials in Vojvodina Province, Serbia. The obtained half-lives were 0.05, 0.23 and 0.15 days for recommended dose application of nicosulfuron, rimsulfuron and prosulfuron, respect­ively. Low residues and short half-life in soil suggested that the risk to sensitive rotational crops after application of those sulfonylurea herbicides is low when they are used in the appropriate dosages.


sulfonylurea herbicide; microwave-assisted extraction; HPLC-UV-DAD; soil, dissipation

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