辅助改善记忆力类保健食品中违禁添加药物检测方法研究

发布时间：2018-03-23 05:34

本文选题：辅助改善记忆　切入点：保健食品　出处：《湖南师范大学》2012年硕士论文　论文类型：学位论文

【摘要】：随着社会竞争压力的不断增大和老年化社会的扩大,辅助改善记忆力类保健品正步入人们的学习工作和日常生活中,相关治疗和预防老年人神经退行性疾病的保健食品种类数目也日益增多。但是由于保健食品中违禁添加药物的现象屡禁不止,而检测方法相对被动滞后,其添加的化学药物的副作用严重影响了人们(尤其是肝、肾功能减弱的中老年人)的身体健康。因此,建立有效、快速的监控手段对提前预防和实时检测违禁添加物的工作具有重要的现实意义。本论文概述了改善记忆力类保健食品的概念及作用、促智药的分类、作用机理和代表药物,通过比较现有常用的违禁药物检测方法,得出高效液相色谱与质谱技术在筛选和检测未知的违禁药物领域所具有的特点及优势。然后利用HPLC-DAD联用、HPLC-MS谱联用的方法测定改善记忆力类保健食品中潜在添加多种违禁药物,比较了不同质谱条件下目标物的响应和特征碎片离子情况,并初步建立了促进记忆力类的化学合成药物相关质谱库,以期达到有效筛选和监控非法添加药物的目的。本论文主要研究工作如下： 1.分析常见的6种益智类药物在不同的质谱条件下的响应情况。6种等摩尔浓度的目标物用不同的流动相(甲醇：水=1：1和乙腈：水=1：1)、流动注射到不同的离子源(ESI源、APCI源及DCBI源),得到相应的质谱图和特征碎片离子,通过比较每个物质的质谱行为的差异性来分析其响应差异的主要原因。 2. HPLC-DAD联用检测辅助改善记忆力类保健食品中12种潜在的促智类药物。优化12种目标物的液相色谱分离条件,根据其目标物的保留值和DAD光谱图能快速、准确的同时测定复杂样品中的疑似违禁添加物,该方法样品处理简单,具有检测限低、可信度高、灵敏度高的特点,应用范围广,可为质量监督部门提供有力依据。 3.建立了HPLC-MS联用检测保健食品中11种钙拮抗剂类药物。通过优化11种钙拮抗剂类药物的液相色谱分离条件和质谱的条件,使目标物具有更好的分离效果和质谱响应值,运用质谱进行定性和定量分析,其结果准确度高、检测限低、灵敏度好,通过解析其质谱裂解规律可为未知样品中添加该类药物或结构衍生物提供参照。 4.建立辅助改善记忆力类药物多级质谱数据库。为建立一种有效的筛选违禁药物添加的方法,本实验室有必要建立一套准确性高,信息丰富的质谱数据库,未知样品可根据这些特征谱图(包括一级、二级及多级质谱图)在缺乏对照品或非法添加了未知化学药的情况下,将所采集的信息搜索相匹配的化学药物,由此可实现短时间内对未知成分进行初步筛选和确认的目的。
[Abstract]:With the increasing competitive pressure in society and the expansion of aging society, health products such as auxiliary memory improvement are stepping into people's study work and daily life. The number of health foods related to the treatment and prevention of neurodegenerative diseases in the elderly is also increasing. The side effects of the addition of chemical drugs seriously affect the health of people, especially the middle and old people with weakened liver and kidney functions. Rapid monitoring is of great practical significance for the prevention and real-time detection of prohibited additives in advance. This paper summarizes the concept and role of memory health food, the classification, action mechanism and representative drugs of antipsychotic drugs. By comparing the commonly used methods for detecting illicit drugs, The characteristics and advantages of high performance liquid chromatography (HPLC) and mass spectrometry in the field of screening and detection of unknown prohibited drugs were obtained. Then, the potential addition of various prohibited drugs in memory improving health foods was determined by HPLC-DAD combined with HPLC-MS. The response and characteristic fragment ions of the target were compared under different mass spectra, and a memory promoting chemosynthetic drug related mass spectrometry library was established in order to screen and monitor the illicit drug addition effectively. The main work of this thesis is as follows:. 1. Analysis of the response of 6 kinds of common probiotics under different mass spectrometry conditions. 6 different mobile phases with equal molar concentrations (methanol: water 1: 1 and acetonitrile: water 1: 1), flow injection into different ion source / ESI source (methanol: water 1: 1) and acetonitrile (acetonitrile: water 1: 1), flow injection into different ion source ESI source. The corresponding mass spectra and characteristic fragment ions were obtained from APCI source and DCBI source. The main reasons for the difference in response were analyzed by comparing the mass spectrum behavior of each substance. 2. Twelve potential intelligence promoting drugs in health food for memory improvement were detected by HPLC-DAD. The liquid chromatographic separation conditions of the 12 target compounds were optimized, and the retention values of the target compounds and the DAD spectrogram were rapidly obtained. The method has the advantages of simple sample treatment, low detection limit, high reliability, high sensitivity and wide application range, which can provide strong basis for quality supervision department. 3. HPLC-MS was used to detect 11 calcium antagonists in health food. By optimizing the separation conditions of 11 calcium antagonists by liquid chromatography and mass spectrometry, the target had better separation effect and mass spectrum response value. The results of qualitative and quantitative analysis by mass spectrometry are of high accuracy, low detection limit and good sensitivity. It can be used as a reference for adding this kind of drugs or structural derivatives to unknown samples by analyzing the cracking law of mass spectrometry. 4. To establish a multistage mass spectrometry database for auxiliary memory improvement drugs. In order to establish an effective method for screening illicit drug additions, it is necessary for our laboratory to establish a highly accurate and informative mass spectrometry database. Unknown samples may search for the collected information on the basis of these characteristic spectra (including primary, secondary and multistage mass spectrometry) in the absence of a reference substance or in the case of the illegal addition of unknown chemicals, to match the collected information, Therefore, the objective of screening and confirming unknown components in a short time can be achieved.
【学位授予单位】：湖南师范大学
【学位级别】：硕士
【学位授予年份】：2012
【分类号】：R155.5;R917

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