本文關(guān)鍵詞：微波等離子體發(fā)射光譜法測定飼料中多元素的方法學(xué)研究　出處：《河北工程大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

  更多相關(guān)文章： 飼料 多元素 微波消解 微波等離子體發(fā)射光譜法

【摘要】：鉀(K)、鈣(Ca)、鈉(Na)、鎂(Mg)、磷(P)、銅(Cu)、鐵(Fe)、錳(Mn)、鈷(Co)、鉬(Mo)等常量和微量元素是維持生物體自身正常生理機(jī)能和新陳代謝所必需的營養(yǎng)成分,其在生長發(fā)育、免疫保護(hù)應(yīng)答等方面的作用不可替代,攝取不足或過量會(huì)導(dǎo)致動(dòng)物體出現(xiàn)代謝障礙、抗病力弱、發(fā)病率高,甚至影響動(dòng)物產(chǎn)品質(zhì)量和危及動(dòng)物生命。因此,飼料中常量和微量元素定量檢測方法受到飼料生產(chǎn)企業(yè)及飼料和畜產(chǎn)品質(zhì)量安全監(jiān)管部門廣泛關(guān)注。近幾年,微波等離子體發(fā)射光譜儀(MP-AES)作為一種新型的原子發(fā)射光譜儀器,具有與電感耦合等離子體發(fā)射光譜儀(ICP-AES)同樣的動(dòng)態(tài)線性范圍寬、分析靈敏度高、多元素分析的優(yōu)勢,同時(shí)可使用氮?dú)庾鳛闅庠?大大節(jié)省了使用成本。且其能進(jìn)行多元素測定分析具有替代火焰原子吸收光譜儀(FAAS)的趨勢。本論文針對典型飼料基體,優(yōu)化了樣品的微波消解前處理?xiàng)l件和MP-AES儀器條件,建立了飼料中K、Ca、Na、Mg、P、Cu、Fe、Mn、Zn、Co、Mo等多元素分析方法,并開展了方法的驗(yàn)證與應(yīng)用,以期為飼料中元素監(jiān)測工作提供準(zhǔn)確、高效的技術(shù)手段。本論文的主要研究內(nèi)容及相關(guān)研究結(jié)果如下:1.飼料中多元素分析的樣品前處理?xiàng)l件優(yōu)化。采用微波消解前處理方法,對微波消解儀的加熱溫度、保持時(shí)間、消解試劑成分以及預(yù)消解分別做了優(yōu)化和對比。結(jié)果顯示,稱取0.3~1.0g飼料樣品,加入6mL硝酸浸泡過夜后加1mL過氧化氫,采用梯度升溫微波消解程序(80℃保持5min、120℃保持5min、190℃保持20min),可以實(shí)現(xiàn)飼料樣品的有效消解。2.飼料中多元素分析的MP-AES方法建立。針對飼料中K、Ca、Na、Mg、P、Cu、Fe、Mn、Zn、Co、Mo等元素,優(yōu)化了MP-AES的泵速、讀取時(shí)間等儀器條件,并對MP-AES法測定各元素的檢出限、線性范圍、標(biāo)準(zhǔn)曲線及其準(zhǔn)確度和精密度等方法學(xué)參數(shù)進(jìn)行了評價(jià)。結(jié)果顯示,11種元素的方法定量限(LOQ)在0.13mg/kg(Mo)~3.37mg/kg(P),標(biāo)準(zhǔn)曲線線性回歸曲線(R2)均大于0.995,平均加標(biāo)回收率在94.9%(K)~118.4%(Mo),復(fù)合飼料質(zhì)控樣(QC-FO-003)的測定結(jié)果均在不確定度范圍內(nèi),表明了此方法的準(zhǔn)確度良好;針對豆粕、魚粉、預(yù)混料和配合飼料,實(shí)驗(yàn)室的日內(nèi)重復(fù)性(相對標(biāo)準(zhǔn)偏差,RSD,n=6)在0%~9.9%,實(shí)驗(yàn)室的日間重復(fù)性(相對標(biāo)準(zhǔn)偏差,RSD,n=4)在0%~8.1%,表明此方法的穩(wěn)定性良好。3.飼料多元素分析的微波消解MP-AES方法驗(yàn)證。利用建立的微波消解MP-AES方法,在5家實(shí)驗(yàn)室對豆粕、魚粉、預(yù)混料和配合飼料等5種典型樣品進(jìn)行了檢測,按科克倫和格拉布斯檢驗(yàn)分析,實(shí)驗(yàn)室間的驗(yàn)證方法重復(fù)性和重現(xiàn)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，

本文編號：1363280