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

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

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1~50μg/kg范围内线性关系良好,定量限为1μg/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。

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.