建立了超高效液相色谱-串联质谱法同时测定食品中香兰素、乙基香兰素、麦芽酚和乙基麦芽酚4种香精的方法。样品用水提取,固相萃取小柱净化,目标化合物采用 UPLCTMBEH C18色谱柱(50 mm×2.1 mm,1.7μm)分离,以甲醇和含0.002 mol/L乙酸铵及0.1%( v/v)甲酸的水溶液为流动相进行梯度洗脱,采用电喷雾离子源电离、正离子多反应监测模式质谱检测。4种香精在5~500μg/L 或10~1000μg/L 质量浓度范围内线性良好,相关系数均在0.9995~0.9998之间;回收率为75.8%~116%,相对标准偏差( RSD,n=6)为1.58%~4.01%。该方法灵敏、准确,检测范围广,分析速度快,适合食品中香兰素、乙基香兰素、麦芽酚和乙基麦芽酚4种香精的检测。
A method has been developed for the simultaneous determination of vanillin,ethyl vanillin,maltol and ethyl maltol in foods by ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry( UPLC-ESI-MS/MS ). The sample was extracted with ultrapure water,and purified with SPE column. The target compounds were sep-arated on a C18 column with the gradient elution of methanol and water containing 0. 002 mol/L ammonium acetate and 0. 1%( v/v)formic acid. The four components were determined in the modes of electrospray positive ionization( ESI+)and multiple reaction monitoring( MRM). The linear ranges were 10—1 000 μg/L for vanillin and maltol and 5—500 μg/L for ethyl vanillin and ethyl maltol,with the correlation coefficients more than 0. 999. The recoveries of the four com-pounds ranged from 75. 8% to 116%,with the relative standard deviations( RSDs)of 1. 58%—4. 01%. The method showed good extraction efficiency,high sensitivity and good reproducibili-ty. It is suitable for the simultaneous detection of vanillin,ethyl vanillin,maltol and ethyl mal-tol in foods.
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