Multi-Residue Pesticide Determination in Flos Chrysanthemi by Mixed Mode SPE Purification with GC-MS/MS Analysis

Abstract

An efficient, fast, and easy-to-perform multi-residue method tracing pesticide residue based on ultrasonic extraction, mixed mode solid-phase extraction for purification and GC–MS/MS analysis was successfully validated and applied to analysis for the simultaneous determination of 100 pesticide residues in traditional Chinese medicine Flos Chrysanthemi samples. Results showed the matrix-matched calibration curve linearity was >0.9900 for all target analytes. The recoveries obtained for each pesticide ranged between 65.3 and 124.7%, and RSD values were less 14.4% for all compounds. The limit of quantification ranged from 0.03 µg · kg⁻¹ to 11.88 µg · kg⁻¹. The proposed method was successfully applied to analysis of 32 commercial chrysanthemum samples collected from cultivation fields in four provinces of China. Most pesticide residue were negative in all samples; 19 pesticide residues were found including acephate, simazine, and carbofuran with a detection rate between 3.1% and 53.1%.

Keywords:

• Chrysanthemum
• GC-MS/MS
• Multi-residue
• Pesticide
• SPE

Acknowledgments

The authors declared no conflict of interest.

This paper was supported by National Science & Technology Major Special Project on Major New Drug Innovation, Item Number: 2009ZX09502-027.

Notes

^a Source c, MRLs for other flowers. http://ec.europa.eu/sanco_pesticides/public/index.cfm?event=commodity.selection.

^b ND, not detected.

^c –, no set MRL value.

^d Source b, MOFCOM: WM/T 2-2004 Green standards of medicinal plants and preparations for foreign trade and economy.