Simultaneous determination of pyrethrins residues in teas by ultra-performance liquid chromatography/tandem mass spectrometry

Abstract

A sensitive and effective method for the simultaneous quantitative determination of pyrethrin residues in teas was developed and validated using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC–MS/MS). The six major constituents of the pyrethrins (pyrethrin I and II, jasmolin I and II, and cinerin I and II) were successfully separated and independently confirmed in a single run within approximately 5 min. The multi-residue analysis of pyrethrins in teas involved simply extraction with acetonitrile, clean-up using a multilayer solid phase extraction cartridge, and subsequent separation by a hydrophilic end-capped Aquasil C18 columns with detection by tandem mass spectrometry using an electrospray ionization source in positive mode (ESI+). Recovery studies were carried out at three spiked levels (0.05, 0.1, 0.5 mg kg −1). The overall average recoveries using this method in green teas and black teas at the three concentration levels ranged from 76.15% to 101.86% with relative standard deviations (RSDs) in the range of 2.71–12.93% ( n = 5) for all analytes. The limits of detections (LODs) were below 0.009 mg kg −1, which were lower than the maximum residue limits (MRLs) of 0.5 mg kg −1 in tea samples established by the European Union legislations in 2008, while the limits of quantification (LOQ) did not exceed 0.03 mg kg −1. This study provides a theoretical basis for China to draw up MRLs for pyrethrins in teas.