UPLC-MS/MS快速鉴定柑橘醋渣中黄酮类成分及其生物活性研究  

Rapid Identification of the Flavonoids from Citrus Vinegar Residue by UPLC-MS/MS and Research on Its Antioxidant Activities

作　　者：张磊 张媛娥 夏辛珂 石松松 付彩霞 雷生姣 ZHANG Lei;ZHANG Yuane;XIA Xinke;SHI Songsong;FU Caixia;LEI Shengjiao(College of Biological and Pharmaceuticals Sciences,China Three Gorges University,Hubei Engineering Research Center for Biological Jiaosu,Yichang 443002,China)

机构地区：[1]三峡大学生物与制药学院,湖北省生物酵素工程技术研究中心,湖北宜昌443002

出　　处：《食品科技》2020年第10期295-301,共7页Food Science and Technology

基　　金：宜昌市应用基础研究项目(A19-302-02);宜昌市科学技术研究与开发项目(A18-201);三峡大学科研项目(HZ2017142,SDHZ2016027)。

摘　　要：通过色谱分离和超高效液相-串联质谱(UPLC-MS/MS)联用技术,对柑橘醋渣中的类黄酮成分进行快速分析与鉴定。采用Hypersil GOLD色谱柱(2.1 mm×100 mm,3μm),以0.5%甲酸水(A)-甲醇(B)为流动相进行梯度洗脱,流速0.2 mL/min,电喷雾(ESI)超高分辨质谱正负离子模式扫描。共分离得到8种化合物,经鉴定为3-O-甲基花旗松素-3-O-芸香糖苷(1)、柚皮素-7-O-葡萄糖苷(2)、芸香柚皮苷(3)、二氢黄酮甙(4)、3-O-甲基花旗松素(5)、枸橘苷(6)、柚皮素(7)、橙皮素(8)。对其中高丰度的化合物3、4、7和8进行生物活性测试,结果表明,化合物7对大肠埃希氏菌的抑制效果最强,最低抑制浓度MIC值为0.016 mg/mL;而在清除1,1-二苯基-2-三硝基苯肼(DPPH)自由基实验中,化合物8的清除效果最好,清除DPPH的半数抑制浓度IC50值为70.29μg/mL。The flavonoids from citrus vinegar residue were quickly analyzed and identified by chromatographic separation and ultra-high performance liquid chromatography-tandem massspectrometry(UPLC-MS/MS).The analysis was carried out on a Hypersil GOLD column(2.1 mm×100 mm,3μm),the gradient elution was carried out with 0.5%formic acid solution(A)-methanol(B)as the mobile phases,and the flow rate was 0.2 mL/min.Electrospray(ESI)ultra-high resolution mass spectrometry was operated in positive and negative ion mode individually.Eight kinds of constituents were isolated from the peeled citrus vinegar residue,which has been identified as 3’-O-methyltaxifolin-3-O-rutinoside(1),naringenin-7-O-glucoside(2),narirutin(3),hesperiden(4),3’-O-methyltaxifolin(5),poncirin(6),hesperetin(7),naringenin(8).The high-abundance compounds 3,4,7 and 8 were tested for antibacterial activity.The results indicated that the four compounds had displayed different repression against three bacterial,and compound 7 had the strongest inhibitory activity against Escherichia coli with a MIC value of 0.016 mg/mL.In the DPPH free radical scavenging experiment,compound 8 had the best scavenging effect,and the half-inhibitory concentration IC50 value of DPPH was 70.29μg/mL.

关 键 词：柑橘醋渣 液相色谱-质谱法(UPLC-MS/MS) 黄酮 抗氧化活性 

分 类 号：O657.63[理学—分析化学]