摘要
目的：建立同时测定饮料和酒类中苯甲酸、糖精钠、脱氢乙酸、甜蜜素、对羟基苯甲酸乙酯和对羟基苯丙酯添加剂的超高效液相色谱串联质谱(UPLC-MS/MS)检测方法。方法样品经超高效C18色谱柱分离,以乙腈：乙酸铵溶液(20 mmol·L-1)为流动相进行梯度洗脱,在质谱负离子模式下进行检测。结果经过系统优化,测得6种食品添加剂在0.1~100μg·mL-1范围内呈现良好的相关性,线性回归系数均大于0.996,其中苯甲酸检出限0.005μg·mL-1；糖精检出限为0.008μg·mL-1,甜蜜素检出限为0.04μg·mL-1,脱氢乙酸检出限为0.003μg·mL-1,对羟基苯甲酸乙酯检出限为0.08μg·mL-1,对羟基苯甲酸丙酯检出限为0.003μg·mL-1,回收率为98.1~102.1％。结论该方法快速、准确、灵敏度高,为饮料中防腐剂和甜味剂检测提供了实用的技术手段。
Objective To establish a UPLC-MS/MS method of detecting benzoic acid, saccharin sodium, dehydrogenation acetic acid, sodium cyclamate, Ethyl p-hydroxybenzoate, Propyl p-hydroxybenzoate simulta-neously in drink and wine. Methods The chromatographic separation was performed on a C18 column with gradient elution, using acetonitrile and ammonium acetate (20 mmol·L-1) as mobile phase. The analyte was de-tected by MS in negative ion mode. Results Under the optimal conditions, the calibration curves of six food additives were a linear in the range of 0.1~100μg/mL-1, with correlation coefficient more than 0.996.The limit of detection was found in the range of 0.005μg·mL-1 for benzoic acid, saccharin sodium for 0.008μg·mL-1, so-dium cyclamate for 0.04μg·mL-1, dehydrogenation acetic acid for 0.003μg·mL-1, ethyl p-hydroxybenzoate for 0.08μg·mL-1, propyl p-hydroxybenzoate for 0.003μg·mL-1. The spiked recoveries were between 98.1~102.1%. Conclusion The method was rapid, accurate, highly sensitive, providing practical techniques for the preser-vatives and sweeteners detection of beverage.
出处
《食品安全质量检测学报》
CAS
2014年第4期1179-1184,共6页
Journal of Food Safety and Quality
关键词
超高效液相色谱-串联质谱
饮料
酒
防腐剂
甜味剂
ultra performance liquid chromatography tandem mass spectrometry
drink
wine
preser-vative
sweetener
