同位素稀释-液相色谱-串联质谱法测定动物源性食品中6种玉米赤霉醇类化合物
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(1.成都市疾病预防控制中心,四川 成都 610041;2.四川大学,四川 成都 610041)

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王炼 男 副主任技师 研究方向为有机污染物残留分析E-mail:septwolvesnjwl@163.com

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中国博士后面上项目资助(2012M521703)


Determination of 6 zeranols residues in animal derived foods by liquid chromatography-tandem mass spectrometry with isotope dilution
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(Chengdu Centre for Disease Control and Prevention,Sichuan Chengdu 610041,China)

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    摘要:

    建立动物源性食品中6种玉米赤霉醇类化合物残留量的同位素稀释-液相色谱-串联质谱的检测方法。方法 样品加入同位素内标后,用甲醇提取,离心后上清液经50 ℃水浴氮气吹至近干,乙酸乙酯溶解残渣后,采用氨基小柱固相萃取,正己烷-乙酸乙酯(20∶80,V/V)和乙酸乙酯两种溶液洗脱后,氮气吹干,流动相溶解后,涡旋混匀过0.22 μm有机滤膜后,LC-MS/MS多反应离子监测(MRM)模式检测,内标法定量。结果 6种玉米赤霉醇类化合物在3类动物源性食品中的加标回收率为84.8%~103.6%;RSD为3.7%~8.6%;检出限和定量限分别为0.03~0.07 μg/kg和0.10~0.24 μg/kg。结论 该方法灵敏、准确,适用于动物源性食品中玉米赤霉醇类物质的检测。

    Abstract:

    To establish a method for determination of 6 zeranols residues in animal derived foods by liquid chromatography-tandem mass spectrometry with isotope dilution.Methods The sample was added isotope internal standard and extracted using methanol. Methanol was nearly dried-up under nitrogen and the residue was dissolved with ethyl acetate. After solid phase extraction of amino cartridge, the eluent was dried-up by nitrogen at 50 ℃. The analytes were dissolved by the mobile phase and determined by liquid chromatography-tandem mass spectrometry. Results The recoveries of analytes were 84.8%-103.6%, and the relative standard deviations of detection were 3.7%-8.6%. The limits of detection and quantification were 0.03-0.07 μg/kg and 0.10-0.24 μg/kg.Conclusion The method is sensitive, accurate and it can meet the determination requirements of 6 zeranols residues in animal derived foods.

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王炼,王希希,张新申.同位素稀释-液相色谱-串联质谱法测定动物源性食品中6种玉米赤霉醇类化合物[J].中国食品卫生杂志,2015,27(5):530-534.

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  • 收稿日期:2015-06-28
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  • 在线发布日期: 2015-11-03
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