超高效液相色谱-串联质谱法同步检测食品中的2-甲基咪唑及4-甲基咪唑  

Simultaneous Determination of 2-Methylimidazole and 4-Methylimidazole in Various Foods by Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：庞美蓉[1] 林钦 戴明 任小英 张英[1] 

机构地区：[1]浙江大学生物系统工程与食品科学学院,浙江省农产品加工技术研究重点实验室,浙江省食品加工技术与装备工程中心,浙江杭州310058 [2]福建省产品质量检验研究院国家加工食品质量监督检验中心,福建福州350002

出　　处：《分析测试学报》2016年第8期943-948,共6页Journal of Instrumental Analysis

基　　金：国家“973”计划项目(2012CB720806);福建省科技厅民生科技专项(2013Y6003)

摘　　要：建立了超高效液相色谱-串联质谱（UPLC-MS/MS）同步检测食品中2-甲基咪唑（2-MEI）和4-甲基咪唑（4-MEI）的分析方法。大多数食品超声提取后可直接进样,基质极其复杂的样品（如酱油、咖啡、茶叶等）需经强阳离子交换柱（PCX）萃取净化,采用同位素内标法定量。在优化条件下,2-MEI和4-MEI的检出限分别可达0.5 ng/g和1.4 ng/g,回收率分别为82.6%～98.1%和89.5%～108.1%,日内相对标准偏差（RSD）分别为1.3%～4.5%和1.0%～5.0%,日间RSD分别为2.0%～5.4%和1.9%～6.5%。采用该方法对市售90余种加工食品进行抽样检测,结果发现2-MEI仅在少量食品中存在且含量较低,而4-MEI在多种食品中存在,含量较高的食品包括老抽酱油（3 224.20～18 795.93 ng/g）、咖啡（0～5 554.35 ng/g）、曲奇（63.48～584.78 ng/g）、焦糖色素饼干（373.12～1 899.60 ng/g）、可乐（44.13～342.77 ng/g）、大麦茶（3131.05～3 335.60 ng/g）等。该文还首次报道了不同品种茶叶（16～761.89 ng/g）中4-MEI的含量。An ultrahigh performance liquid chromatography -tandem mass spectrometric （UPLC - MS/MS） method was developed for the simultaneous determination of 2-methylimidazole （2-MEI） and 4-methylimidazole （4-MEI） in various foods. Most of foods could be injected directly after ultrasonic extraction. Solid phase extraction was needed for extremely complex sample matrix （such as sauce, coffee and tea） , and the target analytes were quantified by isotope internal standard. Under the opti- mized conditions, the limits of detection for 2-MEI and 4-MEI were up to 0. 5 ng/g and 1.4 ng/g, respectively, the recoveries of the method ranged from 82. 6% to 98.1% for 2-MEI and 89.5% to 108.1% for 4-MEI. The intraday RSDs of 2-MEI and 4-MEI were 1.3% -4.5% and 1.0% -5.0% , while their inter-day RSDs were 2.0% -5.4% and 1.9% -6.5% , respectively. The results indica- ted that the method was suitable for simultaneous determination of 2-MEI and 4-MEI in food matrices. This method was applied in more than 90 kinds of foods, in which 2-MEI was only observed in several samples and the contents were relatively low, whereas 4-MEI was detected in most of the tested foods, including clark soy sauce（3 224.20 -18 795.93 ng/g）, coffee（0 -5 554. 35 ng/g）, cookie （63.48 - 584.78 ng/g）, biscuit（ containing caramel, 373.12 - 1 899.60 ng/g）, cola（44. 13 - 342. 77 ng/g） and barley tea（3 131.05 -3 335.60 ng/g）. This study also reported the contents of 4-MEI in different varieties of tea（ 16 -761.89 ng/g） for the first time.

关 键 词：超高效液相色谱-串联质谱(UPLC-MS/MS) 2-甲基咪唑(2-MEI) 4-甲基咪唑(4-MEI) 食品 

分 类 号：O657.63[理学—分析化学] F407.82[理学—化学]