固相萃取-超高效液相色谱/串联质谱同时检测饮料中13种禁限用食品添加剂  

Solid Phase Extraction-Ultra High Performance Liquid Chromatography-Tradem Mass Spectrometry for Simultaneous Determination of 13Restricted Food Additives in Beverages

作　　者：李晶[1,2] 徐济仓[1] 缪明明[1] 周建光[2] 李雪梅[1] 

机构地区：[1]云南烟草科学研究院,云南昆明650106 [2]工业控制技术国家重点实验室,浙江大学智能系统与控制研究所,浙江杭州310058

出　　处：《分析科学学报》2013年第4期488-492,共5页Journal of Analytical Science

基　　金：云南中烟公司科研资助项目(No.2012JC05)

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。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 S sweeteners, 5 preservatives and 5 pigments in beverage samples. The target compounds were separated in 10 minutes on a Waters BEH C18 column（50X2.1 mm,1.7 μm） in gradient elution mode using HPLC methanol and 10 mmol/L ammonium acetate aqueous solution（with 0.1% acetic acid） as mobile phases with a flow-rate of 0.2 mL/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（2-500 μg/L） for the 13 analytes and the detection limits of the analytes were in the range of 0.20-6.79 μg/L. The solid phase extraction was performed on a Waters HLB SPE column with the optimized pretreatment method, the recoveries in spiked samples （10 μg/L, 50μg/L and 100 μg/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 13 food additives in beverage samples simultaneously.

关 键 词：固相萃取 超高效液相色谱-串联质谱法 甜味剂 色素 防腐剂 饮料 

分 类 号：O657.63[理学—分析化学]