摘要
目的:建立测定减肥保健食品中非法添加酚酞和大黄素的高效液相色谱-串联质谱分析方法,并研究其质谱特征,推测其裂解途径。方法:减肥咖啡、减肥茶、减肥胶囊、苹果醋咀嚼片、减肥饼干等不同类型的减肥保健食品经超声波提取15min,以Waters Atlantis T3柱(150mm×2.1mm,3μm)分离后,进行HPLC/MS/MS多反应监测模式下的定性及定量分析。结果:酚酞在0.05～100μg/L的范围内呈良好的线性关系,相关系数为0.9995;大黄素在0.5～100μg/L的范围内呈良好的线性关系,相关系数为0.9991。在低、中、高3个添加水平范围内的平均回收率为70.2%～102.2%;日内精密度均小于8%,日间精密度均小于10%。在检测的24种样品中,检出含有大黄素的样品6个,检出率为25%;含有酚酞的样品16个,检出率为66.7%。结论:方法分析速度快、灵敏度高、回收率高,可用于不同减肥保健食品中非法添加酚酞和大黄素的快速检测。
Objective：To develop a comprehensive analytical method for the determination of phenolphthalein and emodin in the weight-loss functional foods by high performance liquid chromatography tandem mass spectrometry and study mass spectra characterization in order to speculate on fragmentation pathways.Methods：Various weight-loss functional foods,including weight-loss coffee,tea,capsule,chew troche and albumin were extracted under ultrasonication in 15 minutes.Qualitative and quantitative analysis was carried out for the 20 samples under the MRM mode after the chromatographic separation on Waters Atlantis T3（150 mm ×2.1 mm,3 μm）column.Results：Phenolphthalein was linear in the range 0.05～100 μg/L and the linear correlation coefficient reached 0.9995.Emodin was linear in the range 0.5～100 μg/L and the linear correlation coefficient reached 0.9991.The mean recoveries at the three spiked levels（low,middle,high） were 70.2%～102.2%,with the intra-day precision less than 8% and the inter-day precision less than 10%.Emodin was measured in six out of twenty four samples.The detected ratio was 25%.Phenolphthalein was measured in sixteen out of twenty four samples.The detected ratio was 66.7%.Conclusion：The method is reliable,sensitive,high recovery and adapts to the determination of phenolphthalein and emodin in the different weight-loss functional foods.
出处
《食品科技》
CAS
北大核心
2010年第8期339-343,共5页
Food Science and Technology
基金
国家科技支撑计划农业领域课题项目(2006BAD27B02)
关键词
高效液相色谱-串联质谱
酚酞
大黄素
质谱裂解途径
high performance liquid chromatography tandem mass spectrometry
phenolphthalein
emodin
mass spectrum fragmentation pathways
