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目的建立啤酒中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 C_(18)柱(100 mm×2.1 mm,1.7μm)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1.0~200μg/L,标准曲线线性相关系数为0.999 3,检出限为6μg/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。
Objective To establish a method for the determination of 4-methylimidazole in beer by SPE-UHPLC-MS method. Methods The samples were purified by water extraction and purified on a Agala PCX SPE column. The separated samples were separated on a Waters ACQUITY BEH C 18 column (100 mm × 2.1 mm, 1.7 μm) and analyzed by ultra performance liquid chromatography-tandem mass spectrometry (MRM) ) Mode determination, internal standard method. Results The linear range of the method was 1.0 ~ 200μg / L, the standard curve linear correlation coefficient was 0.999 3, the detection limit was 6μg / kg. The spiked recoveries of high, medium and low levels were 88.2% ~ 89.6% with relative standard deviations less than 5%. Conclusion The method is sensitive, rapid and accurate and can be used for the determination of 4-methylimidazole in beer.