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高效液相色谱–四极杆飞行时间质谱法快速筛查饮料中6种人工合成甜味剂
引用本文:杨君,;王建华,;刘靖靖,;李立,;颜冬云. 高效液相色谱–四极杆飞行时间质谱法快速筛查饮料中6种人工合成甜味剂[J]. 化学分析计量, 2014, 0(2): 9-12
作者姓名:杨君,  王建华,  刘靖靖,  李立,  颜冬云
作者单位:[1]青岛大学,山东青岛 266071; [2] 山东出入境检验检疫局,山东青岛266002; [3] 中国检验检疫科学研究院,北京100123
基金项目:国家质检公益性行业科研项目(2012424012-2)
摘    要:建立了高效液相色谱–四极杆飞行时间串联质谱快速检测饮料中糖精钠、甜蜜素、安赛蜜、阿斯巴甜、纽甜、三氯蔗糖6种人工合成甜味剂的方法。样品经水提取,采用C18色谱柱,以甲醇和0.1%甲酸–10 mmol/L甲酸铵溶液为流动相,梯度洗脱,四极杆飞行时间串联质谱电喷雾负离子模式检测。各化合物在0.02~2.0 mg/L范围内均呈现良好的线性关系,相关系数均大于0.998。样品平均添加回收率为63.0%~113.2%,测定结果的相对标准偏差均小于9.6%(n=5)。该方法简便快捷,选择性好,灵敏度高,可满足国内外现行法规的限量要求。

关 键 词:液相色谱–四极杆飞行时间串联质谱  人工合成甜味剂  筛查  饮料

Analysis of 6 Synthetic Sweeteners in Beverage by Liquid Chromatography--Quadrupole Time-of-Flight Mass Spectrometry
Affiliation:Yang Jun, Wang Jianhua, Liu Jingjing, Li Li, Yan Dongyun (1. Qingdao University, Qingdao 266071, China; 2. Shandong Entry-Exit Inspection Quarantine Bureau, Qingdao 266002, China; 3. Chinese Academy of Inspection and Quarantine, Beijing 100123, China)
Abstract:A new method was established for the determination of 6 synthetic sweeteners (sodium saccharin, cyclamate, acesulfame-K, aspartame, neotame, sucralose) in beverage, by using high performance liquid chromatography quadrupole time-of-flight mass spectrometry (HPLC-Q TOF MS). The samples were extracted by water and measured directly by HPLC-Q TOF MS with electrospray ionization in negative mode. The compounds were separated by a C18 column with methyl alcohol and 0.1% formic acid-10 mmol/L ammonium formate solution as the mobile phase. A detailed fragmentation study for 6 synthentic sweeteners was carried out by time of flight. The 6 compounds behave linearly in the range of 0.02-2.0 mg/L with the correlation coefficient of more than 0.998. The recoveries were 63.0%-113.2%, with coefficients of variation below 9.6%(n=5). The method is suitable for routine qualitative and quantitative analyses of synthetic sweeteners in beverage.
Keywords:high performance liquid chromatography-quadrupole time-of-flight mass spectrometry  artificial sweeteners  screening  beverage
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