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  • [Determination of fungicide anilinopyrimidine residues in food by series solid phase extraction-high performance liquid chromatography-tandem mass spectrometry].

[Determination of fungicide anilinopyrimidine residues in food by series solid phase extraction-high performance liquid chromatography-tandem mass spectrometry].

Se pu = Chinese journal of chromatography (2013-01-05)
Dajie Chen, Zhigang Zhang, Yu Zhou, Zongyuan Xiao, Dunming Xu
ABSTRACT

A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/ MS) method was established for the determination of fungicide anilinopyrimidine residues including pyrimethanil, mepanipyrim, and cyprodinil in foodstuffs with series solid phase extraction (SPE). The food sample was first extracted with ethyl acetate, and then purified by an ENVI-Carb cartridge and a Florisil SPE cartridge. The analytes were determined by HPLC-MS/MS and quantified by external standard method. The mass spectrometric detection was operated with electrospray in positive ionization mode and the fungicide anilinopyrimidines were identified in multiple reaction monitoring (MRM) mode. The linear range of the method was 1 - 20 microg/L, with the correlation coefficient (r2) over 0. 999 0. The transitions of the precursor ions to two selected product ions were involved, in which one group for quantification were m/z 200. 1/107. 1 for pyrimethanil, m/z 224. 0/106. 0 for mepanipyrim and m/z 226. 0/108. 1 for cyprodinil, and the other group for identification were m/z 200. 1/183. 1 for pyrimethanil, m/z 224. 0/131. 1 for mepanipyrim and m/z 226. 0/133. 1 for cyprodinil, respectively. No significant matrix effect was found for spiked samples after the purification. The recoveries of the fungicide anilinopyrimidines spiked in food samples were 73.2% -98.7% at the spiked levels of 0. 1, 0.5, 1.0 microg/kg. The relative standard deviations (RSDs) were less than 10%. The limits of detection (LODs) and limits of quantification (LOQs) were 0. 03 microg/kg and 0.1 microg/kg for the three fungicides, respectively. The results showed that the proposed method is sensitive and accurate for the determination of fungicide anilinopyrimidines in foodstuffs. The method should be applicable for routine analysis of pyrimethanil, mepanipyrim, cyprodinil residues in foodstuffs.

MATERIALS
Product Number
Brand
Product Description

Supelco
Mepanipyrim, PESTANAL®, analytical standard
Supelco
Pyrimethanil, PESTANAL®, analytical standard
Supelco
Supel QuE, PSA/C18/ENVI-Carb Tube, pack of 100, AOAC® 2007.01
Supelco
Cyprodinil, PESTANAL®, analytical standard
Supelco
Supel QuE, PSA/ENVI-Carb (EN) Cleanup Tube 2, pack of 100, suitable for EN 15662:2008 per BS
Supelco
Supel QuE, PSA/ENVI-Carb (EN) Cleanup Tube 1, pack of 100, suitable for EN 15662:2008 per BS
Supelco
Supel QuE, PSA/C18/ENVI-Carb Tube, pk of 50, AOAC® 2007.01, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/ENVI-Carb Tube 1, pk of 50, suitable for EN 15662:2008 per BS, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/ENVI-Carb Tube 2, pk of 50, suitable for EN 15662:2008 per BS, centrifuge tube volume 15 mL , Shaker Compatible