Chinese Journal of Chromatography ›› 2016, Vol. 34 ›› Issue (11): 1055-1062.DOI: 10.3724/SP.J.1123.2016.07007

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Rapid screening of 27 pesticide residues in chili powder by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry

LIU Yongqiang, LI Kai, XU Wenjuan, GUO Liqiang, SUN Jun   

  1. Weifang Entry-Exit Inspection and Quarantine Bureau, Weifang 261041, China
  • Received:2016-07-06 Online:2016-11-08 Published:2016-11-03
  • Supported by:

    Program of Shandong Entry-Exit Inspection and Quarantine Bureau (No. SK201613); Weifang Science and Technology Development Plan Project (No. 2015ZJ1101).

Abstract:

An analytical method was established for the simultaneous determination of 27 pesticide residues in chili powder by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS). The samples were extracted with acetonitrile, and cleaned-up by solid phase extraction (SPE) with Carb/NH2 cartridges, and eluted with acetonitrile-ethyl acetate (3: 1, v/v). The eluent was determined by UPLC-Q-TOF/MS with electrospray ionization in positive mode. The confirmatory analysis was carried out by comparing the retention times, accurate masses, isotope abundance and isotope spacing of all the compounds and fragment ions with Targeted MS/MS. The correlation coefficients (r) were greater than 0.997 in the linear ranges of the 27 pesticides. The limits of quantification (LOQs) of the 27 pesticides were 2.5-5.0 μg/kg. At the three spiked levels, the recoveries were between 72.3% and 118.9%, with the relative standard deviations (RSDs, n=6) ranging from 0.21% to 12.7%. The method is efficient, sensitive and accurate, and can meet the requirement of the determination of the 27 pesticides in chili powder.

Key words: chili powder, pesticide residues, screening, ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS)

CLC Number: