亞3色譜技術(shù)在食品藥品非法添加快速檢測(cè)及新成分鑒定中的應(yīng)用
發(fā)布時(shí)間:2018-04-27 00:18
本文選題:非法添加 + 快速檢測(cè)方法; 參考:《廣東藥科大學(xué)》2016年碩士論文
【摘要】:非法添加是近年來(lái)在食品藥品中出現(xiàn)的一種高科技造假行為,嚴(yán)重危害公眾生命健康與社會(huì)和諧穩(wěn)定。液相色譜是非法添加物質(zhì)的主要檢測(cè)技術(shù),目前大部分研究?jī)H針對(duì)有限的幾種目標(biāo)成分,普遍存在監(jiān)督檢驗(yàn)效率低、檢驗(yàn)成本過(guò)高的問(wèn)題,迫切需要開(kāi)發(fā)多成分通用的高通量快速檢測(cè)方法。色譜柱是液相色譜技術(shù)的核心。亞微米色譜柱技術(shù)是最近液相色譜高通量分析方法的研究熱點(diǎn),不僅具有亞微米色譜柱的高效分離性能,還克服了亞微米色譜柱抗污染能力差的缺陷,同時(shí)可直接應(yīng)用于常規(guī)液相色譜系統(tǒng),具有廣闊的應(yīng)用前景。本文以中成藥、保健食品、中藥材及食品中常見(jiàn)的代表性非法添加物作為示范性研究對(duì)象,基于亞色譜技術(shù)開(kāi)展多成分通用的高通量快速檢測(cè)方法。主要內(nèi)容分為以下六部分:第一章對(duì)目前食品藥品非法添加情況、常用檢測(cè)技術(shù)及色譜填料技術(shù)進(jìn)展進(jìn)行綜述,主要分析了非法添加現(xiàn)狀、危害及特點(diǎn),并對(duì)現(xiàn)有常用檢測(cè)技術(shù)與亞色譜技術(shù)在非法添加快速檢測(cè)中的應(yīng)用前景進(jìn)行了分析和討論。第二章建立了壯陽(yáng)類(lèi)中成藥中%種非法添加物同時(shí)快速檢測(cè)的高效液相色譜法與液質(zhì)聯(lián)用確證法。在%內(nèi)實(shí)現(xiàn)所有成分快速分離,線性范圍、回收率及精密度均滿(mǎn)足分析要求。通過(guò)對(duì)批實(shí)際樣品分析,發(fā)現(xiàn)$種非法添加物與種西地那非新衍生物。結(jié)合薄層色譜、柱色譜分離純化技術(shù)與質(zhì)譜及核磁共振結(jié)構(gòu)鑒定技術(shù),確證該衍生物為)*+羥乙基)哌嗪磺酰,正丙氧基苯基-甲基正丙基.吡啶并*/,嘧啶$(.)硫酮。第三章建立了降壓類(lèi)保健食品中種非法添加化學(xué)藥物同時(shí)快速檢測(cè)的高效液相色譜法和液質(zhì)聯(lián)用確證法。在$內(nèi)實(shí)現(xiàn)種成分快速分離,線性范圍、回收率及精密度均滿(mǎn)足分析要求。通過(guò)對(duì)$批實(shí)際樣品分析,發(fā)現(xiàn)種已報(bào)道成分與種沙坦類(lèi)新成分,經(jīng)液質(zhì)聯(lián)用法確證為纈沙坦。第四章建立了肉制品中$種合成色素的高效液相色譜快速分析方法和液質(zhì)聯(lián)用確證法,樣品采用分級(jí)提取思路,結(jié)合固相萃取及分散固相萃取技術(shù)凈化,建立了$種色素同時(shí)快速處理方法。分別在內(nèi)實(shí)現(xiàn)種水溶性色素與種脂溶性色素快速分離,線性范圍、回收率及精密度均滿(mǎn)足分析要求。通過(guò)對(duì)批實(shí)際樣品分析,發(fā)現(xiàn)種非法添加合成色素。第五章建立了穿山甲中藥材中種非法添加色素同時(shí)快速檢測(cè)的高效液相色譜法和液質(zhì)聯(lián)用確證法。在內(nèi)完成種色素分離,線性范圍、回收率及精密度均滿(mǎn)足分析要求。通過(guò)對(duì)批穿山甲中藥材檢測(cè),發(fā)現(xiàn)種新非法添加色素,經(jīng)液質(zhì)聯(lián)用法確證為梔子黃。第六章總結(jié)了亞色譜技術(shù)取得的研究成果與本文的創(chuàng)新點(diǎn)及存在的問(wèn)題。本文首次基于亞色譜技術(shù)建立了食品藥品中多種非法添加成分同時(shí)快速檢測(cè)方法;采用新型分散固相萃取技術(shù)建立脂溶性合成色素快速處理方法;在實(shí)際樣品分析過(guò)程中發(fā)現(xiàn)多種非法添加成分并鑒定出多個(gè)新非法添加物。綜上所述,本論文基于亞色譜技術(shù)建立了類(lèi)非法添加成分同時(shí)快速檢測(cè)方法,與傳統(tǒng)方法相比檢驗(yàn)效率顯著提高,檢測(cè)成本顯著降低,表明該技術(shù)在非法添加高通量快速檢測(cè)方法開(kāi)發(fā)中具有廣闊的應(yīng)用前景,可為有效打擊食品藥品非法添加提供強(qiáng)有力的技術(shù)支撐。
[Abstract]:Illegal addition is a kind of hi-tech counterfeiting behavior in food and drugs in recent years, which seriously endangers the health of the public and social harmony and stability. Liquid chromatography is the main detection technology for the illegal addition of substances. At present, most of the research is only aimed at the limited number of target components, and the efficiency of supervision and inspection is low and the cost of inspection is too high. It is urgent to develop a multicomponent and universal high throughput rapid detection method. Chromatographic column is the core of liquid chromatography. Submicron chromatographic column technology is the focus of recent high throughput analysis of liquid chromatography. It not only has high efficiency of separation of submicron chromatographic column, but also overcomes the deficiency of poor anti pollution ability of submicron chromatographic column. In this paper, the representative illegal additives in Chinese patent medicine, health food, Chinese medicinal materials and food are used as demonstrative research objects. The high flux and rapid detection method of multi components based on sub chromatography is carried out in this paper. The main contents are divided into six parts. Chapter 1: the first chapter reviews the current illegal addition of food and drug, the common detection technology and the progress of chromatographic packing technology, mainly analyzes the status of illegal addition, the hazards and characteristics, and analyzes and discusses the application prospects of the existing detection technology and subchromatographic technology in the illegal addition of fast detection. The second chapter is established. High performance liquid chromatography and liquid chromatography-determination method for simultaneous rapid detection of various illegal additives in Chinese adult Chinese medicine. The rapid separation of all components, linear range, recovery rate and precision are met in%. By analyzing batch actual samples, the illegal additives and new derivatives of sildenafil are found. Layer chromatography, column chromatography separation and purification technology, mass spectrometry and nuclear magnetic resonance structure identification technology, confirmed that the derivative is * + hydroxyethyl) piperazine, n-propane phenyl methyl n-propyl, pyridine and * / pyrimidine $(.) sulfur ketone. The third chapter established a high performance liquid chromatography for the simultaneous rapid detection of chemical drugs in antihypertensive foods. The rapid separation of the species, the linear range, the recovery rate and the precision are satisfied. Through the analysis of the actual samples of the $batch, the new components of the species and the sarartan are found. The fourth chapters have established the high performance liquid phase of the two kinds of synthetic pigments in the meat products. The rapid analysis method of chromatograph and liquid chromatography-determination method, the sample adopts the idea of classification extraction, combined with solid phase extraction and dispersed solid phase extraction technology, to establish a rapid treatment method for the two kinds of pigments. The rapid separation of water soluble pigments and fat soluble pigments is realized, and the linear range, recovery rate and precision are satisfied. In the fifth chapter, a high performance liquid chromatography and a liquid chromatograph confirmatory method were established for the simultaneous rapid detection of pigments in the Chinese medicinal materials of pangolin. The linear range, recovery rate and precision were satisfied. In the sixth chapter, the research results obtained by subchromatograph and the innovation and problems in this article are summarized. In this paper, a new method of simultaneous rapid detection of various illegal additives in food and drugs is established based on the subchromatograph technology; a new type of new method is established for the first time. The fast processing method of fat soluble synthetic pigments was established by the dispersed solid phase extraction technology. In the analysis of actual samples, many illegal additives were found and several new illegal additives were identified. In summary, this paper established a fast speed detection method based on sub chromatographic technique based on sub chromatography technology, and compared with the traditional method. Significantly improved, the detection cost significantly decreased, indicating that the technology has a broad application prospect in the development of illicit high throughput rapid detection methods, and can provide a strong technical support for the effective fight against the illegal addition of food and drug.
【學(xué)位授予單位】:廣東藥科大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2016
【分類(lèi)號(hào)】:R155.5
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本文編號(hào):1808335
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