Citation: 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. doi: 10.3724/SP.J.1123.2015.11040 shu

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

1.
1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
2.
2. Thermo Fisher Scientific Inc., Shanghai 201206, China

Corresponding author: ZHAO Shanzhen,
Received Date: 23 November 2015

Fund Project: 上海市技术性贸易壁垒专项(15TBT005) (15TBT005)上海市科委技术标准专项(15DZ0503201) (15DZ0503201)安徽省科技专项(1604b0602028). (1604b0602028)

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