Using Qu ECh ERS Method and Ultra-high-pressure Liquid Chromatography Tandem Mass Spectrometry to Rapidly Determine Five Sulfonylurea Herbicides in Soil Samples

PENG Xi-tian;XIA Hong;HU Xi-zhou;PENG Li-jun;Qi Zhi-hong;SHEN Jing;Institute of Agricultural Quality Standards and Testing Technology Research , Hubei Academy of Agricultural Science;

ultra-high-pressure liquid chromatography coupled with tandem mass spectrometry;;sulfonylurea herbicides;;multi-residue;;Qu ECh ERS method;;soil

A efficient, rapid and sensitive method of determing 5 sulfonylurea herbicides(nicosulfuron, methsulfuron-methyl,chlorsulfuron, ethametsulfuron-methyl and bensulfuron-methyl) in soil was established. The buffered modified Qu ECh ERS(quick, easy, cheap, effective, rugged and safe) method was used to extract the residues of sulfonylurea herbicides. The extracts were concentrated and redissolved with Me OH / H2O(1 / 1, V / V) to be directly analyzed with ultra-high-pressure liquid chromatography and tandem mass spectrometry(UPLC-MS / MS). Under the optimized LC and MS conditions, the matrix effects(ME) was investigated and obvious signal suppression was observed for all analytes. Matrix-matched calibrations were used to analyze the residues of sulfonylurea herbicides in soil. Results showed that good linearities in the range of 0.2~100.0 μg / kg were obtained for all sulfonylurea herbicides with R2 larger than 0.996 9. The limits of quantitation(LOQs)were found to be in the range of 0.07 ~0.10 μg / kg. The method recoveries of the sulfonylurea herbicides spiked at low,middle and high concentrations in soil samples were from 75.9% to 94.0%, with intra-day and inter-day relative standard deviations less than 11.5%, indicating that the established method has great potential for determing sulfonylurea herbicides in soil samples.