固相萃取-超高效液相色谱-串联质谱法测定啤酒中4-甲基咪唑的含量
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(天津市疾病预防控制中心卫生检测所,天津 300011)

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李建平 男 主管技师 研究方向为食品、环境卫生检验E-mail:LJP100@163.com

通讯作者:

马永民 男 主任技师 研究方向为食品、环境卫生检验E-mail:13662055367@163.com

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Detection of 4-methylimidazole in beer by solid-phase extraction coupled with ultra high performance liquid chromatography-tandem mass spectrometry
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(The Physical and Chemical Laboratory of the Department of Health Detection in Tianjin Centers for Disease Control and Prevention,Tianjin 300011,China)

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    摘要:

    建立啤酒中4-甲基咪唑的固相萃取-超高效液相色谱-串联质谱检测方法。方法 样品经水提取,Agala PCX固相萃取柱净化,经色谱柱Waters ACQUITY BEH C18柱(100 mm×2.1 mm,1.7 μm)分离,超高效液相色谱-串联质谱多反应监测(MRM)模式测定,内标法定量。结果 方法的线性范围为1.0~200 μg/L,标准曲线线性相关系数为0.999 3,检出限为6 μg/kg。高、中、低3个浓度水平的加标回收率为88.2%~89.6%,相对标准偏差小于5%。结论 本方法灵敏、快速、准确,可用于啤酒中4-甲基咪唑的测定。

    Abstract:

    To establish a method for the detection of 4-methylimidazole in beer by solid-phase extraction (SPE) coupled with ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).Methods Samples were extracted by water and purified by Agala PCX solid phase extraction column, then the sample was separated in a Waters ACQUITY BEH C18 column (100 mm×2.1 mm, 1.7 μm). The 4-methylimidazole was determined by UPLC-MS/MS in the multiple-reaction monitoring (MRM) mode and quantified by internal standard. Results The calibration curve had a good linearity in the range of 1.0-200 μg/L with correlation coefficient of 0.999 3. The detection limit was 6 μg/kg. The average recoveries at three spiked levels were in the range of 88.2%-89.6%, and the relative standard derivation was below 5%.Conclusion The method is simple, rapid, sensitive and accurate, which could be used for the detection of 4-methylimidazole in beer.

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李建平,渠志华,王辰,马永民.固相萃取-超高效液相色谱-串联质谱法测定啤酒中4-甲基咪唑的含量[J].中国食品卫生杂志,2016,28(5):610-613.

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  • 收稿日期:2016-06-20
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  • 在线发布日期: 2016-10-18
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