Determination of 106 Pesticide Residues in Citrus Grandis Exocarpium / 中国药学杂志

ABSTRACT

OBJECTIVE: To establish a method for determination of pesticide residues in Citrus Grandis Exocarpium by mass spectrometry. METHODS: After vortex extraction with acetonitrile, the samples were purified with prime-HLB SPE. GC-MS/MS analysis was performed on a DB17 MS(30 m×0.25 mm, 0.25 μm)capillary column with electron impact(EI) source. LC-MS/MS analysis was performed on a Phenomenex Kinetex C18(2.1 mm×100 mm, 2.6 μm) column with gradient elution using water(containing 5 mmol•L-1 ammonium formate and 0.1% formic acid) and 95% acetonitrile(containing 5 mmol•L-1 ammonium formate and 0.1% formic acid). Electrospray ionization(ESI) source was applied by positive ionization in multiple reaction monitoring(MRM) mode. RESULTS: The calibration curves of 106 pesticide residues showed good linearity with correlation coefficients above 0.990 9. The average recoveries for all target compounds fell in the range of 57.6%-134.4%, with RSDs below 15%. Seven kinds of prohibited pesticides and 25 strictly restricted and commonly used ones were detected in 20 batches of samples, which mainly belong to insecticide, acaricide and fungicide. CONCLUSION: The method is fast, accurate and highly sensitive for the screening and confirmation of pesticide residues in Citrus Grandis Exocarpium, which provides a basis for the control of pesticide residues in similar mattrix medicinal plants.