摘要
目的:建立超高效液相-串联四级杆-飞行时间质谱法,用于测定食品中24种酚丁、酚酞及其衍生物。方法:采用超高效液相-串联四级杆-飞行时间液质联用仪,以Waters HSS T31.8μm C_(18)为色谱柱;以0.1%甲酸和甲醇:乙腈(1:1)为流动相;梯度洗脱(0 min,20%A;6 min,95%A;10 min,95%A;10.5 min,20%A;12 min,20%A);流速为0.3 mL/min;Target MS/MS模式;电喷雾离子源正离子模式,扫描范围50~1000。结果:该方法中各组分在0~50μg/mL浓度范围内线性良好,精密度小于3%,各组分回收率为84.2%~97.7%,方法稳定性较好。1批样品检出双辛酚丁,含量为2573 mg/kg;2批样品检出酚酞,含量分别为1538 mg/kg和2054 mg/kg。结论:该方法快速、准确、灵敏度高,进一步完善了减肥及润肠通便食品中非法添加化学物质的检测,为保障食品安全提供技术支持。
Objective:To establish a method by ultra-high performance liquid chromatography/quadrupole time-of-flight-mass spectrometry(UPLC-DAD-Q-TOF-MS/MS)for the detection of 24 kinds of oxyphenisatine,phenolpthalein and their derivatives in food.Methods:The analysis was performed using an UPLC-DAD-Q-TOF-MS/MS system with a Waters HSS T31.8μm C_(18) column.The mobile phase consisted of 0.1%formic acid and a mixture of methanol and acetonitrile(1:1)for gradient elution(0 min,20%A;6 min,95%A;10 min,95%A;10.5 min,20%A;12 min,20%A).The flow rate was set to 0.3 mL/min.Target MS/MS mode was used with electron spray ionization(ESI)positive ionization,and the scanning range was 50–1000.Results:The method showed good linearity in the concentration range of 0–50μg/mL,with relative standard deviations(RSD%)less than 3%.The recovery rates of the components ranged from 84.2%to 97.7%,and the method demonstrated good stability.One batch of samples detected oxyphenisatin diacetate impurity 2 with a content of 2573 mg/kg,and two batches detected phenolphthalein,with contents of 1538 mg/kg and 2054 mg/kg,respectively.Conclusion:This method is fast,accurate,and highly sensitive.It further enhances the detection of illegal chemical additives in weight loss and intestinal laxative foods and provides technical support for ensuring food safety.
作者
赵琪
张珊珊
张超
陈卫
贾昌平
ZHAO Qi;ZHANG Shanshan;ZHANG Chao;CHEN Wei;JIA Changping(Traditional Chinese Medicine Health Products Room,Suzhou Institute for Drug Control,Suzhou 215000,China)
出处
《食品科技》
北大核心
2024年第11期320-326,共7页
Food Science and Technology
关键词
酚丁
酚酞
衍生物
减肥食品
oxyphenisatine
phenolpthalein
derivatives
weight lose food
