摘要
开发了破乳诱导萃取结合电感耦合等离子体质谱(inductively coupled plasma mass spectrometry,ICP-MS)分析鱼油中镉元素的方法。优化了影响破乳萃取效果的关键参数:表面活性剂类型和浓度、HNO3浓度及鱼油取样量,并将所建立的方法应用于实际鱼油样品中镉元素的萃取。破乳萃取法的最优条件为表面活性剂类型为TritonX-114、其浓度为0.10g/mL、HNO3的浓度为5%、鱼油取样量为2.5g。该法对鱼油中镉元素的检出限为0.038μg/kg,往样品中添加镉标准溶液,配置成1、10、100μg/kg三个梯度的加标鱼油样品进行加标回收,添加回收率范围为90.3%~104.9%,RSD均小于3.9%,结果准确可靠。在0~200μg/kg的范围内线性关系良好,标准曲线的相关系数大于0.9999。与微波消解法处理样品相比,2种前处理方法所得结果之间差异不显著(P>0.05)。破乳诱导萃取法是一种操作简单、绿色环保、效率较高的样品前处理方法,与ICPMS相结合能够准确、灵敏地测定鱼油中镉元素的含量。
A method was developed for the analysis of cadmium in fish oil by demulsification-induced extraction and inductively coupled plasma mass spectrometry(ICP-MS).The key parameters affecting demulsification extraction were optimized:surfactant type and concentration,HNO3 concentration and fish oil sampling quantity.The optimal conditions for demulsification extraction method were that the surfactant type was Triton x-114,the concentration was 0.10g/mL,the concentration of HNO3 was 5%,and the sampling amount of fish oil was 2.5g.The detection limit of cadmium in fish oil was 0.038μg/kg.Cadmium standard solution was added to the sample,and labeled fish oil samples with three gradients of 1,10 and 100μg/kg were configured for labeling recovery.The recovery range was 90.3%~104.9%,and RSD was less than 3.9%.The results were accurate and reliable.Good linear relationship was obtained in the range of 0~200μg/kg,the recovery range was 90.3%~104.9%,and the correlation coefficient of the standard curve was greater than 0.9999.Compared with the sample treated by microwave digestion,there was no significant difference between the two methods with pretreatment(P>0.05).Demulsification induced extraction is a simple,green and efficient sample pretreatment method.Combined with ICP-MS,it can accurately and sensitively determine the content of cadmium in fish oil.
作者
柳溪
LIU Xi(Tianjin Institute of Food Safety Inspection Technology,Tianjin 300308)
出处
《中国食品添加剂》
CAS
北大核心
2021年第2期118-122,共5页
China Food Additives
关键词
鱼油
破乳诱导萃取法
电感耦合等离子体
镉
fish oil
demulsification induced extraction
inductively coupled plasma
cadmium
