超高效液相色谱-串联质谱测定饮料和酒中防腐剂与甜味剂
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0.1~100 μg?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0.005 μg?mL-1; 糖精检出限为0.008 μg?mL-1, 甜蜜素检出限为0.04 μg?mL-1, 脱氢乙酸检出限为0.003 μg?mL-1, 对羟基苯甲酸乙酯检出限为0.08 μg?mL-1, 对羟基苯甲酸丙酯检出限为0.003 μg?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 simultaneously 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 detected 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 0.1~100 μg/mL-1, with correlation coefficient more than 0.996.The limit of detection was found in the range of 0.005 μg?mL-1 for benzoic acid, saccharin sodium for 0.008 μg?mL-1, sodium cyclamate for 0.04 μg?mL-1, dehydrogenation acetic acid for 0.003 μg?mL-1, ethyl p-hydroxybenzoate for 0.08 μg?mL-1, propyl p-hydroxybenzoate for 0.003 μg?mL-1. The spiked recoveries were between 98.1~102.1％. Conclusion The method was rapid, accurate, highly sensitive, providing practical techniques for the preservatives and sweeteners detection of beverage.
标题：超高效液相色谱-串联质谱测定饮料和酒中防腐剂与甜味剂
英文标题：Determination of preservative and sweetener in drink and wine by ultra per-formance liquid chromatography tandem mass spectrometry
作者：
王震 徐州市产品质量监督检验中心
石丽珠 徐州市产品质量监督检验中心
中文关键词:超高效液相色谱-串联质谱,饮料,酒,防腐剂,甜味剂,
英文关键词:ultra performance liquid chromatography tandem mass spectrometry,drink,wine,preservative,sweetener,
发表日期：2014-02-28
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