色谱

色谱

• 研究论文 •    下一篇

超高效液相色谱-电喷雾质谱法结合同位素稀释技术检测动物源性食品中的六溴环十二烷异构体

施致雄1,2,封锦芳2,李敬光1,赵云峰1,吴永宁1,2

  

  1. 1.National Institute for Nutrition and Food Safety, Chinese Center for Disease Control and Prevention, Beijing 100050, China;
    2.School of Public Health and Family Medicine,Capital Medical University, Beijing 100069, China
  • 收稿日期:2007-09-17 修回日期:2007-11-06 出版日期:2008-01-30 发布日期:1984-09-25

Analysis of hexabromocyclododecane diastereoisomers in foods of animal origin using ultra performance liquid chromatography-mass spectrometry and isotope dilution

SHI Zhixiong1,2, FENG Jinfang2, LI Jingguang1, ZHAO Yunfeng1, WU Yongning1,2

  

  1. 1.National Institute for Nutrition and Food Safety, Chinese Center for Disease Control and Prevention, Beijing 100050, China;
    2.School of Public Health and Family Medicine,Capital Medical University, Beijing 100069, China
  • Received:2007-09-17 Revised:2007-11-06 Online:2008-01-30 Published:1984-09-25

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摘要：

建立了使用超高效液相色谱-电喷雾四极杆质谱(UPLC-ESI-MS)结合同位素稀释技术准确测定动物源性食品中六溴环十二烷(HBCD)的3种非对映异构体的方法。试样在加入同位素内标13C-HBCD后进行索氏提取,提取液去除脂肪后经硅胶固相萃取柱浓缩、净化后,通过Waters ACQUITY UPLCTM BEH C18色谱柱分离,以甲醇-乙腈混合液和水为流动相进行梯度洗脱。在UPLC-MS分析过程中以保留时间和母离子信息进行定性,选择离子记录(SIR)方式定量。该法对于所测试的鲜奶、鱼肉等样品,检出限为0.1～0.4 ng/g,定量限为0.4～1.2 ng/g。对于加标鱼肉样品,添加水平为0.6,2.0和6.0 ng/g时,3种被测物的加标回收率为92.9%～99.3%,相对标准偏差为3.1%～8.0%。

关键词: 超高效液相色谱, 电喷雾质谱, 六溴环十二烷异构体, 食品 , 同位素稀释

Abstract:

A method for the detection of the α, β and γ-diastereoisomers of hexabromocyclododecane (HBCDs) in foods of animal origin, such as fish, chick, milk, butter etc., was developed using ultra performance liquid chromatography-electrospray ionization mass spectrometry (UPLC-ESI-MS) and isotope dilution. The HBCDs with the spiked isotopic 13C-HBCDs, the internal standards, were extracted using Soxhlet extraction, and further purified using acidic silica treatment and solid phase extraction. The separation of HBCDs was performed on Waters ACQUITY UPLCTM system with the column of BEH C18 and the gradient elution solvent of methanol-acetonitrile and water at a flow rate of 0.2 mL/min. The HBCDs were identified on the basis of the retention times and precursor ions, and quantitatively determined under the selected ion recording mode, m/z 640.7 for the ［M-H］- ion. The limits of detection (LODs) of HBCDs ranged from 0.1 to 0.4 ng/g; and the limits of quantification (LOQs) ranged from 0.4 to 1.2 ng/g. The average recoveries ranged from 92.9% to 99.3% for the spiked levels of 0.6, 2.0 and 6.0 ng/g, with the relative standard deviations (RSDs) between 3.1% and 8.0%.

Key words: electrospray ionization-mass spectrometry (ESI-MS), food , hexabromocyclododecane diastereoisomers, isotope dilution, ultra performance liquid chromatography (UPLC)