本文選題：微波等離子體炬　切入點(diǎn)：質(zhì)譜　出處：《東華理工大學(xué)》2017年碩士論文

【摘要】：在無(wú)需樣品預(yù)處理的情況下,常壓質(zhì)譜分析方法是一種原位、高通量、低耗損、實(shí)時(shí)在線、高靈敏度的質(zhì)譜學(xué)方法。隨著,常壓質(zhì)譜技術(shù)廣泛應(yīng)用,快速分析物質(zhì)的方法變得極其重要。本文主要采用微波等離子體炬電離質(zhì)譜(MPT-MS)新技術(shù)對(duì)金屬元素進(jìn)行分析研究,并開(kāi)拓MPT-MS直接分析有機(jī)物的其它應(yīng)用(如食品安全、刑事偵查、環(huán)境分析等)。本文主要研究?jī)?nèi)容包括以下五個(gè)方面,主要內(nèi)容為:1.系統(tǒng)地介紹了幾種常壓等離子體技術(shù)的基本原理、方法和裝置,重點(diǎn)對(duì)微波等離子體炬質(zhì)譜分析技術(shù)在藥物、石材、食品及環(huán)境等領(lǐng)域的典型應(yīng)用進(jìn)行了述評(píng)。2.采用新型微波等離子體炬四極桿質(zhì)譜(MPT-Q-MS)為實(shí)驗(yàn)平臺(tái),對(duì)四極桿質(zhì)譜儀樣機(jī)進(jìn)行性能測(cè)試,同時(shí)進(jìn)行離子源電離機(jī)理的初步分析。在此基礎(chǔ)之上,發(fā)展了針對(duì)固、液、氣態(tài)樣品的不同進(jìn)樣方式。3.利用微波等離子體炬(MPT)軟電離、無(wú)Ar背景的特性,在四極桿質(zhì)譜儀(Q-MS)和線性離子阱質(zhì)譜儀(LTQ-MS)上進(jìn)行對(duì)比實(shí)驗(yàn)。根據(jù)Q-MS儀器的特性,對(duì)20多種金屬元素進(jìn)行分析研究,并得到水質(zhì)中金屬元素在Q-MS儀器上的初步規(guī)律;但因Q-MS儀器無(wú)串聯(lián)質(zhì)譜功能,為了更好的對(duì)水質(zhì)中金屬元素進(jìn)行分析研究,采用LTQ-MS儀器,在正/負(fù)離子模式下對(duì)金屬元素進(jìn)行分析研究。研究結(jié)果表明:Q-MS儀器對(duì)金屬元素定量分析的檢出限(LOD)能達(dá)到商用LTQ-MS儀器相同的數(shù)量級(jí)(ng·L-1);在Q-MS儀器上金屬元素呈現(xiàn)的質(zhì)譜峰主要為[M]+、[MOH]+、[MO]+,而在LTQ-MS儀器上主要為[M(NO3)a(H2O)b](a-1)+,且LTQ-MS儀器的負(fù)離子模式比正離子模式更適合水質(zhì)中金屬元素的定量分析。4.為了拓展MPT源的應(yīng)用范圍,結(jié)合MPT高溫?zé)嵝?yīng)及電離效應(yīng)。在無(wú)需樣品處理的前提下,采用MPT-LTQ-MS對(duì)食品領(lǐng)域的大米中黃曲霉毒素進(jìn)行快速分析,并對(duì)多種市售大米品質(zhì)進(jìn)行評(píng)價(jià),結(jié)果表明:該方法線性范圍在0.5-20μg·L-1,LOD為0.12μg·L-1。而通過(guò)對(duì)毒物的分析研究發(fā)現(xiàn),MPT-LTQ-MS方法能為刑事偵查提供一種快速定性分析的手段。為了進(jìn)一步擴(kuò)大該方法的應(yīng)用領(lǐng)域,本文還對(duì)農(nóng)產(chǎn)品中蜂蜜里的四環(huán)素進(jìn)行檢測(cè),檢測(cè)的四種市售蜂蜜中四環(huán)素含量均在國(guó)標(biāo)允許范圍類(lèi)。因此,該方法為直接分析有機(jī)樣品提供了一種新的質(zhì)譜分析方法。5.總結(jié)了微波等離子體炬質(zhì)譜新技術(shù)的應(yīng)用成果,展望了其以后的發(fā)展和應(yīng)用。
[Abstract]:In the absence of sample pretreatment, atmospheric mass spectrometry is an in-situ, high-throughput, low-loss, real-time on-line, high-sensitivity mass spectrometry method.With the wide application of atmospheric mass spectrometry, rapid analysis of substances has become extremely important.In this paper, a new technique of microwave plasma torch ionization mass spectrometry (MPT-MS) is used to analyze metal elements, and other applications such as food safety, criminal investigation, environmental analysis and so on are developed for direct analysis of organic matter by MPT-MS.The main content of this paper includes the following five aspects, the main content is 1: 1.The basic principles, methods and devices of several atmospheric pressure plasma techniques are introduced systematically. The typical applications of microwave plasma torch mass spectrometry in the fields of medicine, stone, food and environment are reviewed.Using a new type of microwave plasma torch quadrupole mass spectrometry (MPT-Q-MS) as the experimental platform, the performance of the quadrupole mass spectrometer was tested and the ionization mechanism of the ion source was analyzed.On this basis, different sampling methods for solid, liquid and gas samples have been developed.By using the characteristics of microwave plasma torch (MPT) soft ionization without ar background, a comparative experiment was carried out on a quadrupole mass spectrometer (Q-MS) and a linear ion trap mass spectrometer (LTQ-MS).According to the characteristics of Q-MS instrument, more than 20 kinds of metal elements were analyzed and studied, and the preliminary rules of metal elements in water quality on Q-MS instrument were obtained, but because Q-MS instrument had no series mass spectrometry function,In order to better analyze and study metal elements in water, LTQ-MS instrument was used to analyze metal elements in the mode of positive and negative ions.The results show that the detection limit for quantitative analysis of metal elements by the: Q-MS instrument can reach the same order of magnitude as that of commercial LTQ-MS instruments, and the mass spectra peaks of metal elements in Q-MS instruments are mainly [M], [MOH], [MO], and [M(NO3)a(H2O)b] a-1 in LTQ-MS instruments.The anion mode of LTQ-MS instrument is more suitable for quantitative analysis of metal elements in water than that of positive ion mode.In order to expand the application of MPT source, the high temperature thermal effect and ionization effect of MPT are combined.Without sample processing, aflatoxin in rice in food field was analyzed quickly by MPT-LTQ-MS. The results showed that the linear range of this method was 0.5-20 渭 g / L ~ (-1) and the linear range was 0.12 渭 g / L ~ (-1).It is found that MPT-LTQ-MS method can provide a rapid qualitative analysis method for criminal investigation.In order to further expand the application field of this method, the tetracycline in the honey of agricultural products is also detected. The tetracycline contents in the four kinds of marketable honey are all within the allowable range of the national standard.Therefore, this method provides a new mass spectrometry method for direct analysis of organic samples.The application of microwave plasma torch mass spectrometry is summarized, and its future development and application are prospected.
【學(xué)位授予單位】：東華理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：O657.63

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