亲水相互作用色谱-四极杆/静电场轨道阱高分辨质谱检测奶粉中的氟乙酸钠

基于亲水相互作用色谱-四极杆/静电场轨道阱高分辨质谱系统,建立了奶粉中氟乙酸钠的快速筛查和定量检测方法。奶粉样品用水溶解后经正己烷脱脂,用6 mol/L硫酸调节pH值,经乙腈提取后用亲水相互作用色谱-四极杆/静电场轨道阱高分辨质谱进行分析。结果表明,该方法在1~50 μg/kg范围内线性关系良好,定量限为1 μg/kg,平均回收率为85.5%~106%,相对标准偏差为5.20%~13.6%。该方法可用于配方奶粉、脱脂奶粉和乳清粉等奶粉产品中氟乙酸钠的快速筛查和定量分析。

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

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.