Chinese Journal of Chromatography ›› 2012, Vol. 30 ›› Issue (09): 889-895.DOI: 10.3724/SP.J.1123.2012.04024

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Determination of eight pesticide residues in tea by liquid chromatography-tandem mass spectrometry and its uncertainty evaluation

HU Beizhen1*, CAI Haijiang2, SONG Weihua1   

  1. 1. Shaoxing Entry-Exit Inspection and Quarantine Bureau, Shaoxing 312000, China; 2. Institute of Shaoxing Water Environmental Science Co., Ltd., Shaoxing 312000, China
  • Received:2012-04-16 Revised:2012-07-09 Online:2012-09-28 Published:2012-09-20

Abstract: A method was developed for the determination of eight pesticide residues (fipronil, imidacloprid, acetamiprid, buprofezin, triadimefon, triadimenol, profenofos, pyridaben) in tea by liquid chromatography-tandem mass spectrometry. The sample was extracted by accelerated solvent extraction with acetone-dichloromethane (1:1, v/v) as solvent, and the extract was then cleaned-up with a Carb/NH2 solid phase extraction (SPE) column. The separation was performed on a Hypersil Gold C18 column (150 mm×2.1 mm, 5 μm) and with the gradient elution of acetonitrile and 0.1% formic acid. The eight pesticides were determined in the modes of electrospray ionization (ESI) and multiple reaction monitoring (MRM). The analytes were quantified by matrix-matched internal standard method for imidacloprid and acetamiprid, by matrix-matched external standard method for the other pesticides. The calibration curves showed good linearity in 1~100 μg/L for fipronil, and in 5~200 μg/L for the other pesticides. The limits of quantification (LOQs, S/N>10) were 2 μg/kg for fipronil and 10 μg/kg for the other pesticides. The average recoveries ranged from 75.5% to 115.0% with the relative standard deviations of 2.7%~7.7% at the spiked levels of 2, 5, 50 μg/kg for fipronil and 10, 50, 100 μg/kg for the other pesticides. The uncertainty evaluation for the results was carried out according to JJF 1059-1999 “Evaluation and Expression of Uncertainty in Measurement”. Items constituting measurement uncertainty involved standard solution, weighing of sample, sample pre-treatment, and the measurement repeatability of the equipment were evaluated. The results showed that the measurement uncertainty is mainly due to sample pre-treatment, standard curves and measurement repeatability of the equipment. The method developed is suitable for the conformation and quantification of the pesticides in tea.

Key words: pesticide residues, tea, uncertainty evaluation, liquid chromatography-tandem mass spectrometry (LC-MS/MS)

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