Determination of 12 kinds of pesticide residues in Fritiliariae Thunbergii Bulbus by HPLC-MS / 中草药

ABSTRACT

Objective: To develop an analysis method based on N-propylethylenediamine (PSA)-HPLC-QQQ-MS/MS for the determination of 12 kinds pesticide residues in Fritiliariae Thunbergii Bulbus and to quantify them in 20 batches of Fritiliariae Thunbergii Bulbus produced in various places in Zhejiang province. Methods: Fritiliariae Thunbergii Bulbus samples were extracted with acetonitrile and purified by the small column of PSA. The prepared samples were analyzed by HPLC-QQQ-MS/MS in multiple reaction monitoring (MRM) mode, and the pesticides were qualitified by the internal standard method. Results: All the 12 pesticides showed good linearities in their reasonable range (r = 0.9986-0.9998), and the average recoveries of all the pesticides were in the range of 68.1%-108.0% at three spiked levels of 90, 300, and 900 ng/mL. The RSD values were in the range of 1.1%-6.1%, and the LODs of each pesticide were all in the range of 0.08-1.0 μg/kg. Conclusion: The method is suitable for the multiresidues analysis of pesticides in Fritiliariae Thunbergii Bulbus simultaneously and the quality of Fritiliariae Thunbergii Bulbus is basically good for the safty although it contains a trace of several pesticide residues.