Dalian Ocean University, Dalian, China.
Key Laboratory of Environment Controlled Aquaculture, Ministry of Education, Dalian, China.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2021 Jul;38(7):1096-1104. doi: 10.1080/19440049.2021.1902573. Epub 2021 May 1.
An efficient and simple method for determining vanillin, methyl vanillin and ethyl vanillin in milk and dairy products was developed using a liquid-liquid extraction (LLE) procedure coupled to high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). Different extraction procedures were tested and optimised by spiking three vanillin compounds into a blank matrix in which none of any food additives were detected, and the extraction with acetonitrile solution and -hexane as cleaning sorbent allowed an efficient recovery of 87.6-101.7% with RSDs less than 5%. The limit of detection (LOD) ranged from 6.2 to 20.1 μg/kg. High sensitivity, accuracy and selectivity were found for the in-house validated method, which can eliminate the interferences from complicated matrices effectively, and fulfil the quality criteria for routine laboratory application for real samples. The developed method was then finally applied to screen the three analytes in 65 milk and dairy products including infant formula milk powders from local markets to check for compliance with Chinese Regulation. Concentrations of the total vanillin and ethyl vanillin ranged from 0.0323 to 246.3 mg/kg, which is within the limits of Chinese regulations.
建立了一种高效、简单的牛奶和乳制品中香兰素、甲基香兰素和乙基香兰素的测定方法,采用液液萃取(LLE)结合高效液相色谱-串联质谱(LC-MS/MS)。通过向空白基质中添加三种香兰素化合物进行测试和优化了不同的提取程序,该基质中未检测到任何食品添加剂,乙腈溶液和正己烷作为净化吸附剂的提取方法可实现 87.6-101.7%的高效回收率,相对标准偏差(RSD)小于 5%。检测限(LOD)范围为 6.2-20.1μg/kg。该内部验证方法具有高灵敏度、准确性和选择性,可有效消除复杂基质的干扰,满足常规实验室实际样品应用的质量标准。最后,该方法应用于筛查 65 种牛奶和乳制品中的三种分析物,包括当地市场上的婴儿配方奶粉,以检查是否符合中国法规的要求。总香兰素和乙基香兰素的浓度范围为 0.0323-246.3mg/kg,在中国法规的限量范围内。