Determination of six typical pesticide residues in soybean by dispersive solid-phase extraction-ultra performance liquid chromatography-tandem mass spectrometry
An analytical method for the simultaneous detecting bentazone,acifluorfen,chlorantraniliprole,emamectin benzoate,pyraclostrobin,quizalofop-P-ethyl and its metabolite quizalofop-acid in soybean by ultra-performance liquid chromatography-tandem mass spectrometry was established,which provided an effective tool for monitoring the residue risk of pesticides in soybean.The method was simple,fast,accurate and sensitive.The sample was extracted by 1%formic acid-acetonitrile and purified by dispersive solid phase extraction.The mobile phase was ammonium formate-water solution(containing 0.01%formic acid)and ammonium formate-methanol solution(containing 0.01%formic acid).Phenyl chromatographic column was used for separation,and matrix matching standard curve external standard method was used for quantitative analysis.The results showed that the average recoveries of the target compounds and their metabolites at the spiked levels of 0.001-1 mg/kg ranged from 78.1%to 116.0%,with the relative standard deviations(RSD)ranged from 1.6%to 20.5%.The linear relationships were good in the range of 0.001-1 mg/kg(R2≥0.991 1),and the limits of quantification(LOQs)were 0.001 mg/kg.Furthermore,soybean samples collected from Inner Mongolia were determined by this method.It was found that bentazone,chlorantraniliprole,and pyraclostrobin were detected in soybean,ranging from<0.001 mg/kg to 0.024 mg/kg.The residues of quizalofop-acid,acifluorfen and emamectin benzoate were all lower than 0.002 mg/kg.The six target pesticide residues in soybean samples all meet the safety requirements of the maximum residue limit of pesticides in China.