Magnetic graphitized carbon black based on crystal growth method combined with high-resolution mass spectrometry for screening of 300 pesticide residues in Radix Codonopsis and Angelica sinensis

Abstract

In this study, a high-throughput method for analyzing 300 pesticide residues in Radix Codonopsis and Angelica sinensis was established by liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS) using iron tetroxide loaded graphitized carbon black magnetic nanomaterial (GCB/Fe₃O₄) as the purification material. It was optimized that saturated salt water and 1 % acetate acetonitrile were used as the extraction solution, then the supernatant was purified with 2 g anhydrous CaCl₂ and 300 mg GCB/Fe₃O₄. As a result, 300 pesticides in Radix Codonopsis and 260 in Angelica sinensis achieved satisfactory results. The limits of quantification of 91 % and 84 % of the pesticides in Radix Codonopsis and Angelica sinensis reached 10 μg/kg, respectively. The matrix-matched standard curves ranging from 10 to 200 μg/kg were established with correlation coefficients (R) above 0.99. The pesticides meeting SANTE/12682/2021 accounted for 91.3 %, 98.3 %, 100.0 % and 83.8 %, 97.3, 100.0 % of the total pesticides added in Radix Codonopsis and Angelica sinensis respectively, which were spiked at 10, 20,100 μg/kg. The technique was applied to screen 20 batches of Radix Codonopsis and Angelica sinensis. Five pesticides were detected, three of which were prohibited according to the Chinese Pharmacopoeia (2020 Edition). The experimental results showed that GCB/Fe₃O₄ coupled with anhydrous CaCl₂ exhibited good adsorption performance and could be used for sample pretreatment of various pesticide residues in Radix Codonopsis and Angelica sinensis. Compared with the reported methods for determining pesticides in traditional Chinese medicine (TCM), the proposed method has the advantage of less time-consuming in the clean-up procedure. Furthermore, as a case study on root TCM, this approach may serve as a reference for other TCM.