Simultaneous determination of 114 pesticides in complex Chinese herbal medicine Fritillaria using ordered mesoporous carbon CMK-3 as a reversed-dispersive solid phase extraction sorbent.

Tong Wu,Shanshan Di,Jiao Wang,Xinquan Wang,Changshan Zhao,Huiyu Zhao,Hao Xu,Zhiwei Wang,Peipei Qi

doi:10.1039/d0ra07229j

Abstract

Fritillaria, a traditional Chinese herbal medicine, is classified into many medicinal species and contains numerous complex components. It is thus difficult to simultaneously detect multiple pesticide residues in different Fritillaria species. An easy, reliable, and widely applicable analytical method based on a modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method coupled with LC-MS/MS was developed to solve these problems encountered during pesticide residue analysis in complex Fritillaria matrices. Ordered mesoporous carbon CMK-3 and a primary secondary amine (PSA) were used as efficient purification sorbents by optimization of the QuEChERS process. Systematic method validation was performed for four species of Fritillaria. The matrix effect of pesticides varied among different Fritillaria species, and matrix-matched standard solutions were thus employed for quantitative analysis. The mean recoveries of all pesticides ranged from 88.6% to 95.5%, with mean relative standard deviations (RSD) lower than 6% at spiked concentrations of 30, 120, and 240 μg kg−1. The limits of quantification (LOQ) for the developed method were in the range of 30–120 μg kg−1. This method was further used to analyze 47 Fritillaria samples from Zhejiang province, China, and seven pesticides were detected in 22 Fritillaria samples. These results demonstrate that the developed method is suitable for an accurate analysis of multiple pesticide residues in various Fritillaria.

Highlights

Fritillaria, an important traditional Chinese herbal medicine with antitussive and expectorant properties, is widely used as an ingredient in patented medicines and health foods
When ACN was used as the extraction solvent, all pesticide recoveries were larger than 70%, and 71.1% of the pesticide recoveries were in the range of 90–110%
A modi ed QuEChERS coupled with LC-MS/MS method was developed for the simultaneous determination of 114 pesticides in Fritillaria

Summary

Introduction

Fritillaria, an important traditional Chinese herbal medicine with antitussive and expectorant properties, is widely used as an ingredient in patented medicines (herbal products) and health foods. There are more than 200 different Chinese patented medicines containing Fritillaria for the treatment of cough and phlegm.[1] The expanding demand for herbal products has led to an increase in the cultivation area and export volume of Fritillaria.[2] To improve the yield and quality of Fritillaria, pesticides are inevitably used to prevent pests (e.g., grub, cutworm), diseases (e.g., gray mold, black spot), and weeds during cultivation. Only eight pesticides are currently registered for use on Fritillaria in China These eight pesticides are not enough to prevent all of the diseases and pests on Fritillaria. The abuse of pesticides o en occurs when unregistered pesticides are used by growers, and the abuse of these pesticides in China has led to large amounts of multiple pesticide residues in Fritillaria, which have been con rmed by previous reports.[3,4]

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