FOOD SCIENCE ›› 2009, Vol. 30 ›› Issue (20 ): 350-355.doi: 10.7506/spkx1002-6300-200920078

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UPLC-MS/MS Isotopic Internal Standard Determination of Estradiol Benzoate Residues in Infant Formula Milk Powder

WANG Quan-lin1,ZHANG Ai-zhi1,CHEN Li-ren2   

  1. 1. Ningbo Academy of Product Quality Supervision and Inspection, Ningbo 315041, China;
    2. Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China
  • Received:2009-06-30 Online:2009-10-15 Published:2010-12-29
  • Contact: WANG Quan-lin

Abstract:

UPLC-MS/MS, a highly specific and sensitive method, was successfully developed for determining estradiol benzoate residues in infant formula milk powder. Sample preparation was involved in enzymatic digestion, extraction with methanol and clean-up by solid-phase extraction (SPE) combining C18 and NH2 columns. Estradiol benzoate was detected by ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) in a positive ionization mode and a multiple reaction monitoring (MRM) mode via electrospray ionization (ESI) source and quantitatively determined using nandrolone-d3 as an internal standard. The limit of detection (LOD) and limit of quantification (LOQ) using this method were 0.39 and 0.95 μg/kg for infant formula milk powder respectively. The recovery rates of estradiol benzoate spiked in infant formula milk powder at levels of 4 and 10 μg/kg were ranged from 76.5% to 86.3% with a relative standard deviations in the range of 9.7%-15.2%.

Key words: infant formula milk powder, UPLC-MS/MS, isotopic internal standard method, hormone, estradiol benzoate

CLC Number: