摘要
建立了超高效液相色谱-串联三重四极杆质谱(ultra-performance liquid chromatography-mass spectrometry/mass spectrometry,UPLC-MS/MS)快速筛查和确证饮料中茶碱、咖啡因2种生物碱和糖精钠、安赛蜜、阿斯巴甜、纽甜、爱德万甜、三氯蔗糖6种甜味剂的方法。样品经乙腈-水(20∶ 80, V/V )超声提取,离心,过滤,经超高效液相色谱分离后,在电喷雾离子源的正负离子电离模式下,用多反应监测(multiple reaction monitoring,MRM)方式采集数据,根据保留时间和定性离子对进行定性筛查,根据峰面积和定量离子对进行定量分析。2种生物碱和6种甜味剂的方法检出限(limit of detection,LOD)为0.003~0.5 mg/kg (信噪比S/N≥3),定量限(limit of quantity,LOQ)为0.01~2 mg/kg(S/ N≥10),回收率为92.3%~110.4%,RSD为0.9%~10.8%。在0.001~14.088 μg/mL均有良好的线性,相关系数 r 均大于0.995。该方法快速、简便、准确、灵敏度高,适用于饮料中2种生物碱和6种甜味剂的批量检测。
A new ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with triple quadrupole method was developed in order to determine theophylline,caffeine,saccharin,acesulfame,aspartame,neotame,advantame and sucralose in beverages. Samples were ultrasonically extracted with acetonitrile and water (20∶ 80,v/v ),followed by centrifugation and filtration. The target compound was separated by UPLC,and positive and negative electrospray ionization at multiple reaction monitoring (MRM) mode was applied. Qualitative screening was achieved with retention time and qualitative ions,and peak area and quantitative ions were used for quantification. The results showed that the limit of detection of the method was 0.003-0.5 mg/kg and the limit of quantification was 0.01-2 mg/kg. The average recovery showed a variation from 92.3% to 110.4% and the RSD was 0.9%-10.8%. Besides,a good linear relationship was found in the range of 0.001-14.088 μg/mL target compounds with correlation coefficients being above 0.995. Overall,this method was rapid,simple,sensitive and accurate,which is suitable for batch determination of the 2 alkaloids and 6 sweetening agents in beverages.
作者
刘红
王林
胡博
李丽霞
黄伟
刘芸
LIU Hong;WANG Lin;HU Bo;LI Lixia;HUANG Wei;LIU Yun(Hubei Institute for Drug Control,Wuhan 430075,China;Hubei University of Chinese Medicine,Wuhan 430065,China;College of Chemistry and Molecular Sciences,Wuhan University,Wuhan 430072,China)
出处
《食品与发酵工业》
CAS
CSCD
北大核心
2019年第17期247-251,共5页
Food and Fermentation Industries
关键词
超高效液相色谱-串联质谱
甜味剂
生物碱
饮料
ultra-high performance liquid chromatography-tandem mass spectrometry
sweetening agent
alkaloids
drink
