Validation of Methodology for Determination of Pesticide Residues in Cereals,Oils and Nuts by QuEChERS-GC-MS/MS Method
Objective:To establish and evaluate the QuEChERS-gas-chromatography-mass spectrometry determination of 57 pesticide residues in grains,oilseeds,and nuts.Method:5 g sample was weighed and extracted with 15 mL acetonitrile-acetic acid(the volume ratio is 99 to 1),extracted and purified by QuEChERS,2 mL was blown dry in water bath nitrogen at 40℃,and 1 mL ethyl acetate was added to redissolve,and then passed through a 0.22 μm organic filter membrane and used for instrumental determination.Qualitative and quantitative data were collected in the multi-reaction monitoring mode at the same time,and the ion peak area was used as the ordinate and the concentration of the standard working solution was used as the abscissa to draw the standard curve for quantification,and the detection limit,accuracy and precision of the method were investigated.Result:The results showed that the method was well linear within the concentration range of 0.005 μg·mL-1 to 0.500 μg·mL-1,R2＞0.99.At the detection limit concentration,20 repeated tests were conducted continuously,with recovery rates ranging from 60%to 120%.Six repeated tests were conducted at high,medium,and low concentrations,with a recovery rate from 60.8%to 118.5%.The test results are in line with the requirements of GB/T 27404-2008.Conclusion:The pretreatment method is simple in operation,accurate and efficient in detection process,and its sensitivity and accuracy can meet the detection requirements of agricultural residues,which is suitable for the detection of pesticide residues in cereals,oils and nuts.
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