色谱 ›› 2016, Vol. 34 ›› Issue (4): 397-400.DOI: 10.3724/SP.J.1123.2015.11040

• 研究论文 • 上一篇    下一篇

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

赵善贞1, 伊雄海1, 时逸吟1, 徐牛生2, 张凯元1, 邓晓军1   

  1. 1. 上海出入境检验检疫局, 上海 200135;
    2. 赛默飞世尔科技中国有限公司, 上海 201206
  • 收稿日期:2015-11-23 出版日期:2016-04-08 发布日期:2012-11-16
  • 通讯作者: 赵善贞
  • 基金资助:

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

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

ZHAO Shanzhen1, YI Xionghai1, SHI Yiyin1, XU Niusheng2, ZHANG Kaiyuan1, DENG Xiaojun1   

  1. 1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China;
    2. Thermo Fisher Scientific Inc., Shanghai 201206, China
  • Received:2015-11-23 Online:2016-04-08 Published:2012-11-16
  • Supported by:

    Shanghai Technical Barriers to Trade Item (No. 15TBT005);Technical Standard Item of Shanghai Science and Technology Commission (No. 15DZ0503201);Science and Technology Project in Anhui Province (No. 1604b0602028).

摘要:

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。

关键词: 氟乙酸钠, 奶粉, 亲水相互作用色谱, 四极杆/静电场轨道阱高分辨质谱

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

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