食品科学

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甘油提取结合超高效液相色谱-三重四极杆串联质谱联用技术检测茶叶及副产物中七类化学成分

管梦迪1,郑亚茹2,杨柱林1,李慧敏3,娄华桥1,杨玉冰3,李佳梅3,易伦朝4,胡永丹1,李斯屿1,任达兵1   

  1. 1. 昆明理工大学
    2. 昆明理工大学食品科学与工程学院
    3. 昆明理工大学食品与科学工程学院
    4. 昆明理工大学农业与食品学院
  • 收稿日期:2023-06-16 修回日期:2023-08-28 出版日期:2023-09-19 发布日期:2023-09-19
  • 通讯作者: 任达兵
  • 基金资助:
    云南省科技计划项目

Glycerin-based Extraction Combined with Ultra-high Performance Liquid Chromatography--riple Quadrupole-Tandem Mass Spectrometry for Determining the Contents of Seven Classes of Chemical Constituents in Tea and its By-products

梦迪 管1, 1, 1, 1, 2, 1, 1, Yong-Dan HU 1,bing DaRen   

  • Received:2023-06-16 Revised:2023-08-28 Online:2023-09-19 Published:2023-09-19
  • Contact: bing DaRen

摘要: 以甘油替代甲醇等传统溶剂,结合超声处理进行样本提取,采用超高效液相色谱-三重四极杆串联质谱联用技术对茶叶中的七类化学成分进行定量分析。通过单因素实验,确定最佳提取工艺:甘油含水量50%、固液比1:10、提取时间10 min、提取温度40 ℃。通过优化色谱-质谱分析条件,建立茶叶中儿茶素、酚酸、黄酮、有机酸、氨基酸、生物碱、核苷酸七类共130种物质的定量分析方法。结果表明所建方法具有较高的灵敏度(检测限:0.0004~0.7609 mg/kg)和准确度(回收率:80.10%~119.97%)。实际样本共检出65个化学成分,不同茶叶及副产物中各成分的含量存在较大差异(86622.93~219652.94 mg/kg),其中含量较高的成分包括表儿茶素(2399.42~21207.83 mg/kg)、表没食子儿茶素(1369.47~7934.14 mg/kg)、表儿茶素没食子酸酯(6484.68~26854.46 mg/kg)、表没食子儿茶素没食子酸酯(6484.68~28844.07 mg/kg)、3-没食子酰基奎宁酸(2230.36~14991.11 mg/kg)、茶氨酸(5901.84~14458.35 mg/kg)、咖啡因(6506.29~12017.14 mg/kg)、奎宁酸(5649.48~29529.46 mg/kg)。相比于茶叶样本,茶叶副产物黄片及茶渣也含有较高含量的咖啡因、儿茶素和茶氨酸等高价值成分,表明这些副产物具有进一步的利用价值。

关键词: 茶叶, 化学成分, 甘油, 提取, 质谱法, 定量

Abstract: In the present work, glycerin was used as alternative solvent to the traditional solvents such as methanol to extract different classes of chemical constituents from tea and its by-products. After extraction, ultra-performance liquid chromatography-triple quadrupole tandem mass spectrometry (UPLC-QQQ-MS/MS) was used to quantify seven classes of chemical constituents in tea. The extraction parameters were studied and optimized by single factor experiments, and the best extraction efficiency can be obtained under the following conditions: glycerin water content 50%, solid-liquid ratio 1:10, extraction time 10 min, extraction temperature 40 °C. By Optimizing the conditions of UPLC-QQQ-MS/MS, a quantitation method was established to measuring the contents of 130 substances which included catechins, phenolic acids, flavonoids, organic acids, amino acids, alkaloids and nucleotides. The results of method validation showed that the developed method has high sensitivity (limit of detection: 0.0004~0.7609 mg/kg) and accuracy (recovery: 80.10%~119.97%). A total of 65 chemical constituents were detected in the actual tea samples, and the content of each compound in different types of tea and by-products varied greatly (86622.93 ~ 219652.94 mg/kg). The compounds including epicatechin (2399.42 ~ 21207.83 mg/kg), epigallocatechin (1369.47~7934.14 mg/kg), epicatechingallate (6484.68~26854.46 mg/kg), epigallocatechingallate (6484.68 ~ 28844.07 mg/kg), theogallin (2230.36 ~ 14991.11 mg/kg), theanine (5901.84 ~ 14458.35) mg/kg), caffeine (6506.29-12017.14 mg/kg), quinic acid (5649.48-29529.46 mg/kg) showed relative high contents. Compared with tea samples, the tea by-products including yellow leaves and tea residue also contain higher contents of caffeine, catechin and theanine, indicating the potential value of these by-products.

Key words: Tea, Chemical constituents, Glycerin, Extraction, Mass spectrometry, Quantitation

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