Determination of residual fipronil in chicken egg and muscle by LC-MS/MS

J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Mar 1:1014:31-6. doi: 10.1016/j.jchromb.2016.01.041. Epub 2016 Feb 2.

Abstract

A simple, sensitive and reliable method was developed and applied to the residue analysis of fipronil in chicken egg and muscle by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Chicken egg and muscle samples were extracted with acetronitrile, then salting out by dehydration with anhydrous magnesium sulfate and sodium chloride. The extracts were purified by the C18 solid phase extraction cartridge prior to analysis by LC-MS/MS. The matrix-matched calibration curve showed a good linear within the concentration range from 0.01 to 2.00μgkg(-1) (r(2)≥0.999). The average recoveries of fipronil at three spiked levels of 0.01, 0.1 and 1.0μgkg(-1) ranged from 79.7% to 98.0%, and the relative standard deviations were less than 8.8%. The decision limit (CCα) and detection capability (CCβ) of fipronil in chicken egg and muscle matrices were all 0.002μgkg(-1) and 0.01μgkg(-1), respectively. The method has also been successfully applied to monitoring fipronil in the real samples.

Keywords: Chicken; Egg; Fipronil; Liquid chromatography–tandem mass spectrometry; Residue.

Publication types

  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Animals
  • Chickens* / metabolism
  • Chromatography, High Pressure Liquid / methods*
  • Eggs / analysis*
  • Insecticides / analysis*
  • Limit of Detection
  • Muscles / chemistry*
  • Pyrazoles / analysis*
  • Solid Phase Extraction / methods
  • Tandem Mass Spectrometry / methods*

Substances

  • Insecticides
  • Pyrazoles
  • fipronil