摘要
目的建立利用热裂解衍生气相色谱-三重四极杆质谱法(gas chromatography triple quadrupole mass spectrometry,GC-MS/MS)测定食品中维生素A的方法。方法食品中维生素A经超声波法提取,提取液用乙腈沉淀蛋白质并用氯化钠分层后,上层有机相过0.22μm有机滤膜过滤。维生素A由于其热不稳定性发生热裂解,产生衍生物二氢猕猴桃内酯,采用气相色谱-三重四极杆质谱法(gas chromatography triple quadrupole mass spectrometry,GC-MS/MS)多反应监测模式(multiple reaction monitoring,MRM)对二氢猕猴桃内酯的定性离子和定量离子进行检测。结果维生素A在0.1~5μg/mL浓度范围内线性关系良好,标准曲线r 2>0.999,方法的相对标准偏差为3.6%~7.2%,乳粉中维生素A的回收率为97.4%~115.8%,维生素A空白药品的回收率为90.4%~95.4%,检出限为0.02μg/mL,定量限为0.1μg/mL。结论该方法可同时对食品中的维生素A进行定性定量分析,精密度和检出限能满足实际检测要求,可用于食品中维生素A的日常测定。
Objective To establish a method for the determination of vitamin A in food by pyrolysis derivatization gas chromatography triple quadrupole mass spectrometry.Methods Vitamin A in food was extracted by ultrasonic method.Protein was precipitated by acetonitrile and separated by sodium chloride.The upper organic phase was filtered by 0.22μm organic filter membrane.The derivative dihydroactinidide was produced by thermal decomposition of vitamin A due to thermal instability.Qualitative and quantitative ions of dihydrokiwifruit lactone were detected by gas chromatography triple quadrupole mass spectrometry(GC-MS/MS)with multi reaction monitoring mode(MRM).Results The linear range of vitamin A in this method was 0.1‒5μg/mL,the linear relationship was good in the concentration range,the standard curve r 2>0.999,the relative standard deviation of the method was 3.6%‒7.2%,the recovery rate of vitamin A in milk powder was 97.4%‒115.8%,and the recovery rate of vitamin a blank drug was 90.4%‒95.4%.The detection limit was 0.02μg/mL,and the limit of quantitation was 0.1μg/mL.Conclusion This method can be used for qualitative and quantitative analysis of vitamin A in food at the same time.The precision and detection limit can meet the actual detection requirements,and can be used for the daily determination of vitamin A in food.
作者
李少鹏
黄濒漩
刘聪熠
马路凯
刘袆帆
LI Shao-Peng;HUANG Bin-Xuan;LIU Cong-Yi;MA Lu-Kai;LIU Hui-Fan(Henan Institute of Product Quality Supervision and Inspection,Zhengzhou 450000,China;Zhongkai Agricultural Engineering College,Guangzhou 510000,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2021年第4期1281-1290,共10页
Journal of Food Safety and Quality
基金
2020年广东省科技创新战略(“攀登计划”)专项资金立项项目(pdjh2020b0291)。
关键词
气相色谱-三重四极杆质谱法
热裂解衍生
二氢猕猴桃内酯
维生素A
gas chromatography triple quadrupole mass spectrometry
pyrolysis derivatization
dihydroactini dide
vitamin A
