食品科学 ›› 0, Vol. ›› Issue (): 0-0.

• 成分分析 •    下一篇

UPLC-MS/MS测定葡萄酒中29种单体酚方法的建立

杨志伟1,王圣仪2,齐鹏宇1,张昂1,张进杰3,王飞1,李响4   

  1. 1. 秦皇岛出入境检验检疫局
    2. 秦皇岛市出入境检验检疫局技术中心
    3. 秦皇岛海关
    4. 秦皇岛海关技术中心
  • 收稿日期:2019-01-10 修回日期:2019-10-29 出版日期:2019-12-25 发布日期:2019-12-24
  • 通讯作者: 张昂 E-mail:zhanganggrape@hotmail.com
  • 基金资助:
    国家重点研发计划“食品安全关键技术研发”重点专项;质检总局科技计划项目

Establishment of UPLC-MS/MS Method for Determination of 29 Monophenols in Wine Abstract

YANG Zhi-wei Sheng-Yi WANG 2,Ang Zhang 2,Wang-Fei 2   

  • Received:2019-01-10 Revised:2019-10-29 Online:2019-12-25 Published:2019-12-24
  • Contact: Ang Zhang E-mail:zhanganggrape@hotmail.com
  • Supported by:
    This work was supported by the National Key Research and Development Program of China;General Administration of Quality Supervision, Inspection and Quarantine (AQSIQ) Science and Technology Plan

摘要: 目的:超高效液相色谱串联质谱技术建立同时测定葡萄酒中29种单体酚的快速检测方法。方法:样品经过酸化甲醇水稀释高速离心后取上清液进样分析,使用ACQUITY UPLC?BEH C18色谱柱洗脱分离,流动相为0.1 %甲酸乙腈和0.1 %甲酸水,电喷雾式离子源负离子模式,多反应检测;离子源温度(TEM):500 ℃;电喷雾电压(IS):-4500 V;气帘气(CUR):40 psi;碰撞气:Medium;雾化气:60 psi;辅助加热气:50 psi,分析时间17 min。结果:29种单体酚的定量限在0.001 mg/L ~ 0.01 mg/L之间,线性相关系数R2均大于0.999,加标回收率在90% ~ 105%之间,RSD在0.26 ~ 7.13之间,结论:该方法前处理简便、灵敏度高、分析时间短,精密度和准确性良好,可用于葡萄酒中29种单体酚的同时检测。

关键词: 单体酚, 葡萄酒, 超高效液相色谱串联二级质谱(UPLC-MS/MS)

Abstract: To establish a rapid method for simultaneous determination of 29 phenols in wine by UPLC-MS/MS. Methods: Samples after acidification methanol water dilution after high-speed centrifugal supernatant sample analysis, using the ACQUITY UPLC?; C18 chromatographic column and elution separation of mobile phase was 0.1% acetonitrile formate and 0.1% formic acid water, electric spray ion source negative ion mode, the reaction detection; Ion source temperature(TEM) : 500 ℃; Electrospray voltage (IS) : -4500 V; Air curtain gas (CUR) : 40 psi; Collision gas: Medium; Atomized gas: 60 psi; Auxiliary heating: 50 psi, analysis time 17 min. Results: The quantitative limit of 29 monomer phenols was between 0.001 mg/L and 0.01 mg/L, the linear correlation coefficient R2 was greater than 0.999, the standard recovery was between 90% and 105%, and the RSD was between 0.26 and 7.13. Conclusion: This method was characterized by simple operation, high sensitivity, fast analysis and short time. This method also has good precision and accuracy and can be applied to detect 29 monophenols in wine.

Key words: Mono-phenolic compounds, Wine, UPLC-MS/MS

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