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当前位置: 首页 > 文章 > UPLC-MS-MS检测饮料中的4-甲基咪唑及其同分异构体2-甲基咪唑 食品科学 2014,35 (8) 244-248
Position: Home > Articles > Determination of 4-(5-)-Methylimidazole and Its Isomer 2-Methylimidazole in Beverage by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry FOOD SCIENCE 2014,35 (8) 244-248

UPLC-MS-MS检测饮料中的4-甲基咪唑及其同分异构体2-甲基咪唑

作  者：
张璐;孔祥虹;何强;李建华;邹阳;李莹
单  位：
陕西出入境检验检疫局
关键词：
超高效液相色谱-串联质谱;4-甲基咪唑;2-甲基咪唑;固相萃取;饮料
摘  要：
建立超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLCMS-MS)法检测饮料中的4-甲基咪唑(4-(5-)-methylimidazole,4-Mel)及2-甲基咪唑(2-methylimidazole,2-Mel)的方法。以水溶解样品,OASIS?MCX固相萃取柱富集净化后,进入UPLC-MS-MS检测,内标法定量。在优化的条件下,以ACQUITY UPLC?HILIC色谱柱(2.1 mm×100 mm,1.7?m)为分析柱,乙腈和5 mmol/L甲酸铵溶液为流动相,在电喷雾正离子多反应监测模式进行检测。结果表明,4-Mel和2-Mel在9~500 ng/mL范围内线性关系良好。方法的定量限为3.0?g/kg。在4个加标水平下,3种不同基质饮料中4-Mel和2-Mel的平均回收率分别为97.3%和93.7%,相对标准偏差分别为3.8%和3.4%,该方法适用于饮料中4-Mel和2-Mel的检测。利用该方法对市售饮料中4-Mel和2-Mel的含量进行检测,在软饮料、焦糖色饮料及咖啡饮料中检出含有4-Mel或2-Mel;而功能性饮料中未检出4-Mel和2-Mel。
译  名：
Determination of 4-(5-)-Methylimidazole and Its Isomer 2-Methylimidazole in Beverage by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry
作  者：
ZHANG Lu;KONG Xiang-hong;HE Qiang;LI Jian-hua;ZOU Yang;LI Ying;Shaanxi Entry-Exit Inspection and Quarantine Bureau;
关键词：
ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS-MS);;4-(5-)-methylimidazole;;2-methylimidazole;;solid phase extraction(SPE);;beverage
摘  要：
An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS) method was developed for the determination of 4-(5-)-methylimidazole(4-Mel) and its isomer, 2-methylimidazole(2-Mel), in beverage. Samples were diluted with water. An OASIS? MCX solid phase extraction column was used to purify and concentrate the target analytes. Under the optimal conditions, the analytes were separated by a Waters ACQUITY UPLC? HILIC column(2.1 × 100 mm, 1.7 ?m) using a mobile phase consisting of acetonitrile and 5 mmol/L ammonium acetate aqueous solution. The analytes were detected in multiple-reaction monitoring(MRM) mode via positive electrospray ionization(ESI+). The results showed that the calibration curves of 4-Mel and 2-Mel were of good linearity in the range of 9–500 ng/mL. The limit of quantification of the method was 3.0 ?g/kg. The average recovery was 97.3% and 93.7% at four spiked levels(3.0, 25, 50 and 75 ?g/kg) for 4-Mel and 2-Mel, respectively, and the relative standard deviation(RSD) was 3.8% and 3.4%, respectively. These figures of merit indicated that the developed method can be used for the determination of 4-Mel and 2-Mel in beverage samples. This method was applied to different beverages. 4-Mel or 2-Mel was found in soft drink, caramel colored beverage and coffee. Contrarily, neither of them was found in energy drinks.

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