new method of determination and confirmation for four pesticide residues in Citrus grandis‘Tomentosa’was developed by HPLC-MS/MS. The sample was extracted with acetonitrile, and purified with a Carbon/NH2 SPE column, then washed with the gradient elution of acetonitrile and 5 mmol aqueous ammonium acetate. At last, the identification of target compounds were measured through MS under multiple reaction monitoring (MRM) mode. The results showed that when the amount of pesticide residues was in the range of 5-200 μg/L, it obtained good linear relation, and its relative coefficient was above 0.99. The detection limit was between 0.1-0.5 μg/kg. When the additional level was at 10-200 μg/kg, the recycle degree was in the range of 81.9%-94.1%, and the relative standard deviation was 5.4%-9.2%. This method
possessed simple operation and accurate result, which could meet the requirements for the determination of pesticides in C.grandis‘Tomentosa’. |