亚3色谱技术在食品药品非法添加快速检测及新成分鉴定中的应用

发布时间：2018-04-27 00:18

  本文选题：非法添加 + 快速检测方法　； 参考：《广东药科大学》2016年硕士论文

【摘要】：非法添加是近年来在食品药品中出现的一种高科技造假行为,严重危害公众生命健康与社会和谐稳定。液相色谱是非法添加物质的主要检测技术,目前大部分研究仅针对有限的几种目标成分,普遍存在监督检验效率低、检验成本过高的问题,迫切需要开发多成分通用的高通量快速检测方法。色谱柱是液相色谱技术的核心。亚微米色谱柱技术是最近液相色谱高通量分析方法的研究热点,不仅具有亚微米色谱柱的高效分离性能,还克服了亚微米色谱柱抗污染能力差的缺陷,同时可直接应用于常规液相色谱系统,具有广阔的应用前景。本文以中成药、保健食品、中药材及食品中常见的代表性非法添加物作为示范性研究对象,基于亚色谱技术开展多成分通用的高通量快速检测方法。主要内容分为以下六部分:第一章对目前食品药品非法添加情况、常用检测技术及色谱填料技术进展进行综述,主要分析了非法添加现状、危害及特点,并对现有常用检测技术与亚色谱技术在非法添加快速检测中的应用前景进行了分析和讨论。第二章建立了壮阳类中成药中%种非法添加物同时快速检测的高效液相色谱法与液质联用确证法。在%内实现所有成分快速分离,线性范围、回收率及精密度均满足分析要求。通过对批实际样品分析,发现$种非法添加物与种西地那非新衍生物。结合薄层色谱、柱色谱分离纯化技术与质谱及核磁共振结构鉴定技术,确证该衍生物为)*+羟乙基)哌嗪磺酰,正丙氧基苯基-甲基正丙基.吡啶并*/,嘧啶$(.)硫酮。第三章建立了降压类保健食品中种非法添加化学药物同时快速检测的高效液相色谱法和液质联用确证法。在$内实现种成分快速分离,线性范围、回收率及精密度均满足分析要求。通过对$批实际样品分析,发现种已报道成分与种沙坦类新成分,经液质联用法确证为缬沙坦。第四章建立了肉制品中$种合成色素的高效液相色谱快速分析方法和液质联用确证法,样品采用分级提取思路,结合固相萃取及分散固相萃取技术净化,建立了$种色素同时快速处理方法。分别在内实现种水溶性色素与种脂溶性色素快速分离,线性范围、回收率及精密度均满足分析要求。通过对批实际样品分析,发现种非法添加合成色素。第五章建立了穿山甲中药材中种非法添加色素同时快速检测的高效液相色谱法和液质联用确证法。在内完成种色素分离,线性范围、回收率及精密度均满足分析要求。通过对批穿山甲中药材检测,发现种新非法添加色素,经液质联用法确证为栀子黄。第六章总结了亚色谱技术取得的研究成果与本文的创新点及存在的问题。本文首次基于亚色谱技术建立了食品药品中多种非法添加成分同时快速检测方法;采用新型分散固相萃取技术建立脂溶性合成色素快速处理方法;在实际样品分析过程中发现多种非法添加成分并鉴定出多个新非法添加物。综上所述,本论文基于亚色谱技术建立了类非法添加成分同时快速检测方法,与传统方法相比检验效率显著提高,检测成本显著降低,表明该技术在非法添加高通量快速检测方法开发中具有广阔的应用前景,可为有效打击食品药品非法添加提供强有力的技术支撑。
[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.

【学位授予单位】：广东药科大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：R155.5
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本文编号：1808335