Determination of sodium fluoroacetate in milk powder by hydrophilic interaction chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

doi:10.3724/SP.J.1123.2015.11040

Abstract

Abstract:

A method for the determination of sodium fluoroacetate in milk powder by hydrophilic interaction chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry was developed. After the sample was dissolved by water, sodium fluoroacetate was degreased by hexane. The pH value of the extractant was adjusted by 6 mol/L H₂SO₄. After extracted by acetonitrile, the extractant was determined by hydrophilic interaction chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry. The linear range of the sodium fluoroacetate was from 1 to 50 μg/kg, with the correlation coefficients greater than 0.99. By detecting the spiked samples, the limits of quantification were 1 μg/kg, while the recoveries were in the range of 85.5%-106% with the relative standard deviations (RSDs) between 5.20% and 13.6%. This method can be used for the quick determination of sodium fluoroacetate in powder formula, skimmed milk powder and whey powder.

Key words: hydrophilic interaction chromatography, milk powder, quadrupole/orbitrap high resolution mass spectrometry (HR-MS), sodium fluoroacetate

CLC Number:

O658

ZHAO Shanzhen, YI Xionghai, SHI Yiyin, XU Niusheng, ZHANG Kaiyuan, DENG Xiaojun. Determination of sodium fluoroacetate in milk powder by hydrophilic interaction chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry[J]. Chinese Journal of Chromatography, 2016, 34(4): 397-400.

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