高效液相色谱-离子阱-飞行时间质谱法定性分析蜂蜜中的黄酮类未知物  

Qualitative analysis of unknown flavanoids in honey by high performance liquid chromatography-ion trap-time of flight tandem mass spectrometry

作　　者：牛之瑞 冯雷 胡赠彬 谭建林 田浩 申玲玲 NIU Zhi-Rui;FEN Lei;HU Zeng-Bin;TAN Jian-Lin;TIAN Hao;SHEN Ling-Ling(Yunnan Institute of Product Quality Supervision & Inspection, Nationnal Agricultural and Sideline Products Quality Supervision and Inspection Center, Kunming 650223, China;Institue of Agro-Products Processing Science and Technology, Yunnan academy of agricultural Sciences, Kunming 650223, China;Shimadzu Global COE, Shimadzu (China) Co., Ltd., Guangzhou 510010, China)

机构地区：[1]云南省产品质量监督检验研究院,国家热带农副产品监督检验中心,昆明650223 [2]云南省农业科学院农产品加工研究所,昆明650223 [3]岛津企业管理(中国)有限公司,广州510010

出　　处：《食品安全质量检测学报》2018年第23期6210-6215,共6页Journal of Food Safety and Quality

基　　金：云南省质量技术监督局科技计划项目(2017ynzjkj01)~~

摘　　要：目的建立高效液相色谱-离子阱-飞行时间串联质谱法(high performance liquid chromatography-ion trap-time of flight tandem mass spectrometry,HPLC-MS-IT-TOF)定性分析蜂蜜中的未知黄酮类物质的分析方法。方法通过查阅相关资料,推断该未知物可能是黄酮类物质,用质谱检测可知与其他干扰物质是否分离。在确定干扰物质与未知黄酮进行分离后,可以得到未知黄酮类物质的分子离子峰和三级质谱碎片,根据碎片离子,推导出了裂解途径,并使用分子式软件预测了未知黄酮类物质的分子式。结果综合实验结果,最后定性了蜂蜜中的未知黄酮类物质为"短叶松素",其分子式为C15H12O5。用超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)将黄酮类未知物质与短叶松素标准品的保留时间、离子对m/z 271.06>253.10和m/z 271.06>191.00及离子比率进行比对,确证定性结果是准确的。结论本实验为蜂蜜中黄酮类未知物定性提供了一个有效的思路和方法。Objective To establish a method for qualitative analysis of unknown flavonoids in honey by high performance liquid chromatography-ion well-flight time series mass spectrometry. Methods By referring to relevant data, that the unknown substance maight be flavonoid, and whether it was separated from other interfering substances could be determined by mass spectrometry. The molecular ion peaks and tertiary mass spectrum fragments of unknown flavonoids could be obtained after the separation of the interfering substance and unknown flavonoids was confirmed. According to the fragment ions, the cracking pathway was deduced, and the molecular formula of unknown flavonoids was predicted by using molecular formula software. Results Based on the results of the comprehensive experiment, the unknown flavonoid in honey was determined as "Pinobanksin", and its molecular formula was C 15 H 12 O 5 . The retention time of unknown flavonoids and the standard compound of Pinobanksin, the ionic ratio of m/z 271.06 > 253.10, m/z 271.06 > 191.00 and the ionic ratio were compared by ultra-high performance liquid chromatography-tandem mass spectrometry, and the confirmed qualitative result was accurate. Conclusion This study provides an effective method for the determination of unknown flavonoids in honey.

关 键 词：短叶松素 黄酮类未知物 高效液相色谱-二极管阵列检测器-离子阱-飞行时间串联质谱法 超高效液相色谱-串联质谱法 

分 类 号：S896.1[农业科学—特种经济动物饲养] O657.63[农业科学—畜牧兽医]