【摘要】 建立了固相萃取-超高效液相色谱/电喷雾电离串联质谱(SPE-UPLC-MS/MS)同时测定饮料中13种禁限用食品添加剂(甜味剂、防腐剂和色素类物质)的分析方法。样品经过OASIS HLB固相萃取小柱萃取净化后,以0.2mL/min的流速,在WatersBEH C18(50×2.1mm,1.7μm)色谱柱上进行快速分离,流动相为10mmol/L乙酸铵(含0.1%乙酸)和甲醇。根据检测物质的性质,利用不同电离模式(ESI-和ESI+),采用多反应监测模式(MRM)进行测定,在2～500μg/L的范围内,各物质线性相关系数均大于0.990,13种检测物质的检出限为0.20～6.79μg/L;利用Waters HLB固相萃取小柱对目标物质进行萃取,对固相萃取条件进行优化后,10、50、100μg/L三个添加水平下平均回收率为85.6%～110.4%,相对标准偏差(RSD)均小于10%(n=5)。所建立的方法简便,灵敏度高,可以满足对饮料中多种不同食品添加剂的同时测定。更多还原

【Abstract】 In this work,an ultra-high performance liquid chromatography-mass spectrometry/mass spectrometry(UPLC-MS/MS)method was established for the separation and determination of 13 restricted food additives,including 3sweeteners,5preservatives and 5pigments in beverage samples.The target compounds were separated in 10minutes on a Waters BEH C18column(50×2.1mm,1.7μm)in gradient elution mode using HPLC methanol and 10mmol/L ammonium acetate aqueous solution(with 0.1%acetic acid)as mobile phases with a flow-rate of 0.2mL/min at 35℃,and were then confirmed and quantified by mass spectrum via positive electrospray ionization(ESI+)for pigments and via negative electrospray ionization(ESI-)for sweeteners and preservatives.Under multiple reaction monitoring(MRM)mode,regression equations revealed acceptable linearity(correlation coefficients>0.990)across the working-standard range(2-500μg/L)for the 13analytes and the detection limits of the analytes were in the range of 0.20-6.79μg/L.The solid phase extraction was performed on a Waters HLB SPE column with the optimized pretreatment method,the recoveries in spiked samples(10μg/L,50μg/L and 100μg/L)ranged from 85.6%to 110.4% with the relative standard deviations less than 10%(n=5).With the advantages of accessibility,high sensitivity and good reproducibility,this simple method can be used to separate and determine 13food additives in beverage samples simultaneously.更多还原