摘要
目的:利用超高效液相色谱-串联质谱技术同时测定干红葡萄酒中18 种花色素单体。方法:将酒样用5%酸化甲醇溶液(含1%甲酸,V/V)稀释500 倍后,滤液经Phenyl-Hexyl色谱柱梯度洗脱,电喷雾离子源正离子模式检测,多反应监测,气帘气压力30 psi,离子喷雾电压5 500 V,离子源温度500 ℃,分析时间20 min。结果:18 种花色素单体在10.0、20.0、50.0 μg/L添加水平的加标回收率在95%~100%之间,R2大于0.999,相对标准偏差在1.71%~2.87%之间,检出限在0.2~3.5 μg/L之间,定量限在0.4~11.5 μg/L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,可用于干红葡萄酒中18 种花色素单体的同时检测。
Objective: To simultaneously determine 18 anthocyanin monomers in red wine using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods: Wine samples were diluted 500 times with acidified methanol solution containing 1% formic acid(V/V) before being filtrated. The filtrate was separated by gradient elution chromatography on a phenyl-hexyl column. Detection was carried out using an electrospray ionization source in the positive ion mode with multiple reaction monitoring(MRM). The mass spectrometric conditions were as follows: curtain gas 30 psi, ion spray(IS) voltage 5 500 V, and ion source temperature 500 ℃. The analysis took 20 min. Results: The recoveries of the analytes at spiked levels of 10.0, 20.0 and 50.0 μg/L were between 95% and 100%, and the calibration curve for each analyte exhibited a correlation coefficient(R^2) of greater than 0.999. The precision, expressed as relative standard deviation(RSD), ranged between 1.71% and 2.87%. The limits of detection(LOD) were between 0.2 and 3.5μg/L, and the limits of quantitation(LOQ) were between 0.4 and 11.5μg/L. Conclusion: This method was characterized by simple pretreatment, high sensitivity, short analysis time, shorter time and good precision and accuracy and could be applied to detect individual anthocyanins in red wine.
作者
金刚
杨志伟
王圣仪
王昶森
马雯
张进杰
张昂
张军翔
JIN Gang;YANG Zhiwei;WANG Shengyi;WANG Changsen;MA Wen;ZHANG Jinjie;ZHANG Ang;ZHANG Junxiang(School of Wine, Ningxia University, Yinchuan 750021, China;Engineering Research Center of Grape and Wine, Ministry of Education, Ningxia Grape and Wine Research Institute,Ningxia Engineering and Technology Research Center of Grape and Wine, Yinchuan 750021, China;Inspection and Quarantine Technique Centre, Qinhuangdao Entry-Exit Inspection and Quarantine Bureau, Qinhuangdao 066004, China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2019年第18期229-235,共7页
Food Science
基金
宁夏回族自治区重点研发计划重大项目(2016BZ06)
质检总局科技计划项目(2017IK253)
宁夏高等学校科研项目(NGY2016066)
关键词
花色素单体
干红葡萄酒
超高效液相色谱-串联质谱
monomer anthocyanin
red wine
ultra performance liquid chromatography-tandem mass spectrometry