微波等离子体发射光谱法测定饲料中多元素的方法学研究

发布时间：2018-01-01 06:15

  本文关键词：微波等离子体发射光谱法测定饲料中多元素的方法学研究　出处：《河北工程大学》2017年硕士论文　论文类型：学位论文

  更多相关文章： 饲料 多元素 微波消解 微波等离子体发射光谱法

【摘要】：钾(K)、钙(Ca)、钠(Na)、镁(Mg)、磷(P)、铜(Cu)、铁(Fe)、锰(Mn)、钴(Co)、钼(Mo)等常量和微量元素是维持生物体自身正常生理机能和新陈代谢所必需的营养成分,其在生长发育、免疫保护应答等方面的作用不可替代,摄取不足或过量会导致动物体出现代谢障碍、抗病力弱、发病率高,甚至影响动物产品质量和危及动物生命。因此,饲料中常量和微量元素定量检测方法受到饲料生产企业及饲料和畜产品质量安全监管部门广泛关注。近几年,微波等离子体发射光谱仪(MP-AES)作为一种新型的原子发射光谱仪器,具有与电感耦合等离子体发射光谱仪(ICP-AES)同样的动态线性范围宽、分析灵敏度高、多元素分析的优势,同时可使用氮气作为气源,大大节省了使用成本。且其能进行多元素测定分析具有替代火焰原子吸收光谱仪(FAAS)的趋势。本论文针对典型饲料基体,优化了样品的微波消解前处理条件和MP-AES仪器条件,建立了饲料中K、Ca、Na、Mg、P、Cu、Fe、Mn、Zn、Co、Mo等多元素分析方法,并开展了方法的验证与应用,以期为饲料中元素监测工作提供准确、高效的技术手段。本论文的主要研究内容及相关研究结果如下:1.饲料中多元素分析的样品前处理条件优化。采用微波消解前处理方法,对微波消解仪的加热温度、保持时间、消解试剂成分以及预消解分别做了优化和对比。结果显示,称取0.3~1.0g饲料样品,加入6mL硝酸浸泡过夜后加1mL过氧化氢,采用梯度升温微波消解程序(80℃保持5min、120℃保持5min、190℃保持20min),可以实现饲料样品的有效消解。2.饲料中多元素分析的MP-AES方法建立。针对饲料中K、Ca、Na、Mg、P、Cu、Fe、Mn、Zn、Co、Mo等元素,优化了MP-AES的泵速、读取时间等仪器条件,并对MP-AES法测定各元素的检出限、线性范围、标准曲线及其准确度和精密度等方法学参数进行了评价。结果显示,11种元素的方法定量限(LOQ)在0.13mg/kg(Mo)~3.37mg/kg(P),标准曲线线性回归曲线(R2)均大于0.995,平均加标回收率在94.9%(K)~118.4%(Mo),复合饲料质控样(QC-FO-003)的测定结果均在不确定度范围内,表明了此方法的准确度良好;针对豆粕、鱼粉、预混料和配合饲料,实验室的日内重复性(相对标准偏差,RSD,n=6)在0%~9.9%,实验室的日间重复性(相对标准偏差,RSD,n=4)在0%~8.1%,表明此方法的稳定性良好。3.饲料多元素分析的微波消解MP-AES方法验证。利用建立的微波消解MP-AES方法,在5家实验室对豆粕、鱼粉、预混料和配合饲料等5种典型样品进行了检测,按科克伦和格拉布斯检验分析,实验室间的验证方法重复性和重现性良好。
[Abstract]:K, K, Ca, Na, mg, P, Cu, Fe, mn, Co). Mo-Mo) and other constants and trace elements are essential nutrients to maintain the normal physiological function and metabolism of organisms, and their role in growth and development, immune protection response and other aspects can not be replaced. Inadequate or excessive intake of animals will lead to metabolic disorders, weak disease resistance, high incidence, and even affect the quality of animal products and endanger animal life. The quantitative detection method of constant and trace elements in feed has been paid more and more attention by feed production enterprises and the quality and safety supervision department of feed and animal products in recent years. Microwave plasma emission spectrometer (MP-AESs) is a new type of atomic emission spectrometer. It has the same dynamic linear range as inductively coupled plasma emission spectrometer (ICP-AESV), high analytical sensitivity and multi-element analysis, and can use nitrogen as a gas source at the same time. It can be used as a substitute for flame atomic absorption spectrometer (Faas). This paper aims at typical feed matrix. The pretreatment conditions of microwave digestion and the conditions of MP-AES instrument were optimized. The method of Mo and other multi-element analysis was verified and applied in order to provide an accurate method for the monitoring of elements in feed. The main research contents and related results of this paper are as follows: 1. Optimization of sample pretreatment conditions for multi-element analysis in feed. Microwave digestion pretreatment method was adopted. The heating temperature, retention time, digestion reagent composition and pre-digestion of microwave digestion apparatus were optimized and compared respectively. After immersing in 6 mL nitric acid for the night and adding 1 mL hydrogen peroxide, the microwave digestion procedure was used to keep the temperature at 80 鈩，

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