超高效液相色谱-串联质谱法同时测定客家娘酒中的2-甲基咪唑、4-甲基咪唑及5-羟甲基糠醛

Simultaneous determination of 2-methylimidazole,4-methylimidazole and 5-hydroxymethylfurfural in Hakka rice wine by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法同时测定客家娘酒中的2-甲基咪唑(2-methylimidazole,2-MEI)、4-甲基咪唑(4-methylimidazole,4-MEI)和5-羟甲基糠醛(5-hydroxymethylfurfural,5-HMF)的分析方法。方法样品经过直接稀释法和标准加入法分别进行前处理,使用ACQUITY UPLC BEH HILIC(100mm×2.1 mm,1.7μm)色谱柱进行样品分离,以甲醇-5 mmol/L氨水为流动相进行梯度洗脱,采用电喷雾离子源正离子模式和多反应监测模式进行检测。结果在优化条件下,2-MEI和4-MEI在1~500ng/mL范围内线性关系良好,相关系数(r^(2))为0.9998和0.9998,5-HMF在50~8000 ng/mL线性范围内r^(2)为0.9970。2-MEI、4-MEI和5-HMF在低、中、高3个浓度添加水平下的回收率范围分别为88.7%~108.0%、77.5%~102.0%和95.7%~98.4%,相对标准偏差分别为4.16%~10.50%、2.04%~5.49%和3.10%~6.62%。2-MEI、4-MEI和5-HMF的检出限分别为3、3和17 ng/mL,定量限分别为10、10和50 ng/mL。结论本方法操作简便、线性关系良好、回收率高,适用于客家娘酒中2-MEI、4-MEI和5-HMF的检测。

Objective To establish an analytical method for simultaneous determination of 2-methylimidazole(2-MEI),4-methylimidazole(4-MEI) and 5-hydroxymethylfurfural(5-HMF) in Hakka rice wine by ultra performance liquid chromatography-tandem mass spectrometry.Methods Samples were pretreated by direct dilution method and standard addition method,respectively,ACQUITY UPLC BEH HILIC(100 mm×2.1 mm,1.7 μm) chromatographic column was used for sample separation,methanol-5 mmol/L ammonia was used as the mobile phase for gradient elution,electrospray ion source positive ion mode and multiple reaction monitoring mode were used for detection.Results Under the optimal conditions,the linear relationships of 2-MEI and 4-MEI were good in the range of 1-500 ng/mL,the correlation coefficients(r^(2)) were 0.9998 and 0.9998,and the linear range of 5-HMF was 50-8000 ng/mL,r^(2) was 0.9970.The recovery ranges of 2-MEI,4-MEI and 5-HMF were 88.7%-108.0%,77.5%-102.0% and 95.7%-98.4% at the low,medium and high levels,respectively,with relative standard deviations of 4.16%-10.50%,2.04%-5.49% and 3.10%-6.62%,respectively.The limits of detection for 2-MEI,4-MEI,and 5-HMF were 3,3,and 17 ng/mL,respectively,and the quantitation limits were 10,10,and 50 ng/mL,respectively.Conclusion This method is simple,with good linear relationship and high recovery rate,and is suitable for the determination of 2-MEI,4-MEI and 5-HMF in Hakka rice wine.