超高效液相色谱-串联质谱同时检测甜味剂和色素类物质.docVIP

  超高效液相色谱-串联质谱同时检测甜味剂 和色素类物质# 李晶1,2，徐济仓1，杨叶昆1，缪恩铭1，李雪梅1** 5 10 15 20 25 30 35 40 （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） 摘要：本研究工作建立了超高效液相色谱－电喷雾电离串联质谱（UPLC－ESI MS/MS）同 时测定香精香料中甜味剂和色素类物质的分析方法。实验采用 Waters BEH C18 (1.7 μm, 2.1 mm×50 mm)色谱柱为分离固定相，采用 10 mmol/L 乙酸铵（含 0.1% 乙酸）和色谱级甲醇 为流动相，以 0.2 mL/min 的流速在 35的柱温下，可以在 10 min 内完成 3 种甜味剂和 5 种 色素的基线分离。在 ESI-负离子模式（甜味剂）和 ESI+正离子模式(色素)下，采用多反应监 测模式进行测定，8 种检测物质的检出限为 0.9～12.0 μg/L；对前处理方法进行优化后，平 均回收率为 82.9%-118.2% ，RSD 均小于 6%(n=5)。所建立的方法简单易操作，灵敏度高， 可以满足对香精香料中甜味剂以及色素类物质的同时测定。 关键词：超高效液相色谱-串联质谱法；甜味剂；色素；香精香料；检测 中图分类号：O657.7+2 Simultaneous Determination of Sweeteners and Pigments by Ultra High Performance Liquid Chromatography-Mass spectrometry/Mass spectrometry LI Jing1,2, Xu Jicang1, Yang Yekun1, Miao Enming1, Li Xuemei1 (1. Yunnan Academy of Tobacco Science , Kunming, 650106, China; 2. State Key Laboratory of Industrial Control Technology, Institute of Cyber-Systems and Control, Zhejiang University, Hangzhou, 310058, China) Abstract: In this work, an ultra high performance liquid chromatography-mass spectrometry/ mass spectrometry (UPLC-MS/MS) method was established for the separation of 3 sweeteners and 5 pigments in flavor and fragrant samples. The target compounds were separated in 10 minute on a Waters BEH C18 column (1.7 μm, 2.1 mm×50 mm) in gradient elution mode using HPLC methanol and 10 mmol/L ammonium acetate aqueous solution (with 0.1% (V/V)) acetic acid) as mobile phases with a flow-rate of 0.2 mL/min at 35℃, and confirmed and quantified by mass spectrum via positive electrospray ionization (ESI+) for pigments and via negative electrospray ionization (ESI-) for sweeteners. Under multiple reaction monitoring (MRM) mode, regression equations revealed acceptable linearity (correlation coefficients=0.9900~0.9999) across the working-standard range (20-500 μg/L) for the 8 analytes and the detection limits of the analytes were in the range of 0.9 μg/L to 12 μg/L). With the optimized pretreatment