鱼肝油中维生素D3 、香精香料及重金属的检测方法研究

发布时间：2018-09-14 17:13

【摘要】：鱼肝油是鳕鱼鲨鱼等鱼类肝脏中提取的脂肪类物质,含有丰富的维生素,不饱和脂肪酸,其作为营养补充剂被人们服用,本文从维生素、香精、重金属三个方面评价鱼肝油品质:传统方法检测鱼肝油维生素D3操作繁琐,本文建立了超高效合相色谱法来检测鱼肝油维生素D3含量,样品经正己烷直接提取,选用Waters 1-AA色谱柱,流动相为80%CO2和20%甲醇,等度洗脱,方法检出限为1.2 mg/kg;定量限为5 mg/kg。维生素D3的平均加标回收率为89.1%,相对标准偏差(RSDs)0.3-3.2%,该方法简单,灵敏,能快速检测鱼肝油中维生素含量。为了掩盖鱼肝油的鱼腥味通常会添加香精,然而有些香精对人体有害,本文使用气相色谱串联质谱法(GC-MS/MS)首次建立了鱼肝油中8种禁用的香精香料的检测方法,样品正己烷超声辅助提取,考察了3种常见的净化方法:固相萃取(SPE)、改良的QuEChERS法、膜过滤净化法;最终确定净化方法膜过滤净化法。该方法首次建立鱼肝油样品中香精香料的检测,该方法灵敏,高效,适用于鱼肝油中香精的检测。本文使用电感耦合等离子质谱法(ICP-MS)检测了鱼肝油中Cu、As、Cd、Pb重金属元素,样品加硝酸和过氧化氢,经微波消解后定容,经ICP-MS进行分析。首次建立鱼肝油样品的ICP-MS方法,该方法灵敏度,适合鱼肝油样品中重金属元素检测。
[Abstract]:Cod liver oil is a fatty substance extracted from the liver of fish such as cod and shark. It is rich in vitamins and unsaturated fatty acids. The quality of cod liver oil was evaluated in three aspects: the traditional method for the detection of cod liver oil vitamin D3 was complicated. A super high efficiency phase chromatography was established to detect the content of cod liver oil vitamin D 3. The samples were extracted directly by hexane. Waters 1-AA column was used with mobile phase of 80%CO2 and 20% methanol. The detection limit of the method was 1.2 mg/kg; and the quantitative limit was 5 mg/kg.. The average recoveries of vitamin D _ 3 were 89.1 and the relative standard deviation (RSDs) was 0.3-3.2. The method was simple and sensitive, and could be used for rapid determination of vitamins in cod liver oil. In order to cover up the fishy smell of cod liver oil, however, some flavours are harmful to human body. In this paper, gas chromatography-tandem mass spectrometry (GC-MS/MS) was used to establish a method for the detection of eight forbidden flavors in cod liver oil for the first time. Ultrasonic assisted extraction of n-hexane from samples was carried out and three common purification methods were investigated: improved QuEChERS method for solid phase extraction (SPE), membrane filtration purification method, and final determination of membrane filtration purification method. The method is sensitive, efficient and suitable for the determination of flavoring in cod liver oil. The heavy metal elements of Cu,As,Cd,Pb in cod liver oil were determined by inductively coupled plasma mass spectrometry (ICP-MS). The samples were treated with nitric acid and hydrogen peroxide. After microwave digestion, the contents of Cu,As,Cd,Pb were determined by ICP-MS. The ICP-MS method for the determination of heavy metals in cod liver oil samples was established for the first time. The method is sensitive and suitable for the determination of heavy metals in cod liver oil samples.
【学位授予单位】：沈阳化工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：R927.1

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