高效液相色谱-离子阱-飞行时间质谱法快速筛查饮料中植物源性成分

Rapid Screening and Confirmation of Plant-Derived Ingredients in Beverage by High Performance Liquid Chromatography-Ion Trap-Time of Flight Mass Spectrometry

采用高效液相色谱-离子阱-飞行时间质谱对饮料中生物碱、皂苷和有机酸等24种植物源性成分进行快速筛查、定性识别和准确定量。样品经高速离心,过0.22μm水系滤膜后,以C_(18)色谱柱(2.1 mm×250 mm,3.0μm)分离,乙腈-0.1%甲酸溶液为流动相进行梯度洗脱,正、负离子模式同时扫描。结果表明,24种化合物在50~750μg/L范围内呈良好的线性关系,相关系数均大于0.995。样品中各化合物的检出限(以信噪比不小于3计)为8~20μg/L。在3种添加量(70、250、700μg/L)条件下,其平均回收率为63.0%~126.6%,相对标准偏差为4.11%~14.73%。该方法利用精确质量数匹配和自建标准库检索,实现快速筛查,并使用多级特征碎片离子进行确证,具有快速、高效、准确等优点,适用于饮料中多种植物源性成分的快速筛查和测定。

A high performance liquid chromatography-ion trap-time of flight mass spectrometry method was used for rapid screening,confirmation and quantification of24alkaloids,saponins and organic acid in beverage.After centrifugation of samples at high speed and filtration through a0.22μm drainage membrane filter,the filtrate was separated on a C18column(2.1mm×250mm,3.0μm)using a binary solvent system composed of acetonitrile and water containing0.1%of formic acid through gradient elution.The analysis was carried out both in the positive and negative ion modes.The results showed that good linear relationships were obtained in the range of50-750μg/L for all24compounds with correlation coefficients of higher than0.995.The limits of detection(LOD)obtained at signal-to-background noise of3for all analytes were in the range of8-20μg/L.Average recoveries were between63.0%and126.6%at three spiked levels(70,250and700μg/L)with relative standard deviations(RSDs)of4.11%-14.73%.Depending on the match of accurate mass number and retrieval in the self-built standard library,rapid screening was achieved and multistage characteristic fragments were also used for confirmation.The method,thanks to its rapidity,high efficiency,and good accuracy,could be used in the rapid screening and determination of multi-plant derived ingredients in beverage.