DCBI-MS法快速筛查保健食品和中成药中违禁药物

发布时间：2018-04-24 16:25

本文选题：解吸附电晕束离子化 + 离子阱质谱　；参考：《湖南师范大学》2013年硕士论文

【摘要】：目前,对保健食品和中成药中违禁药物进行检测多依靠液相色谱、高效液相色谱-质谱联用法等,这些方法测定前需对样品进行前处理,耗时较长,在实际大批量商品筛选时不可操作。敞开式离子化技术成为质谱技术的研究热点和前沿领域,此技术可在无需样品预处理的条件下对复杂基体样品中的痕量待测物进行直接离子化,极大的提高了质谱分析的效率。本文以市场上常见的保健食品和中成药对研究对象,利用实验室自行研制的解吸附电晕束离子化技术对其中可能添加的违禁药物进行快速检测,并研究了快速初筛过程中的基质效应。其主要内容如下： 1.综述保健食品和中成药中违禁药物的添加现状以及对消费者造成的危害。通过与常用的违禁药物检测方法比较,研究常压直接离子化技术在违禁药物检测领域具有的优势。 2.在优化的实验条件下,利用解吸附电晕束离子源(DCBI)结合离子阱质谱快速检测了3个磷酸二酯酶5(PDE5)抑制剂伐地那非、西地那非、他达拉非。采用一级质谱筛选,二级质谱确证,对样品中非法添加物进行定性鉴别；通过二级特征碎片离子进行半定量分析,与传统高效液相色谱-紫外(HPLC-UV)检测法作对比,研究了3个PDE5抑制剂的二级质谱裂解规律。实现了分析速度快、样品用量少、无需使用其他化学试剂、无污染的检测。 3.在优化的实验条件下,建立了DCBI-MS法快速检测9种β2-受体激动剂。利用一级质谱筛选,二级质谱确证,对样品中非法添加物进行定性鉴别；并通过二级特征碎片离子进行半定量分析。本方法无需复杂的前处理过程,简便、快速、灵敏度高,可用于止咳平喘类药物中β2-受体激动剂违禁添加的快速定性及半定量检测。 4.以市场上常见违禁添加的抗疲劳保健食品为研究对象,选取不同剂型的空白样品(片剂,丸剂,胶囊,合剂,酒剂,糖浆,口服液),通过空白加标法测定基质对3个PDE5抑制剂伐地那非、西地那非、他达拉非的检测限及半定量分析的影响。此研究结果为DCBI-MS法测定不同剂型不同辅料中其他目标物的前处理过程的必要性提供了参考依据。
[Abstract]:At present, the detection of illegal drugs in health food and Chinese patent medicine mostly depends on liquid chromatography, high performance liquid chromatography-mass spectrometry and so on. In the actual mass selection of goods can not be operated. The open ionization technology has become the hot spot and frontier of mass spectrometry technology. This technology can directly ionize trace samples in complex matrix samples without sample pretreatment, which greatly improves the efficiency of mass spectrometry analysis. In this paper, the common health food and Chinese patent medicine in the market were used to detect the possible illegal drugs by using the desorption corona beam ionization technology developed by the laboratory. The matrix effect in the process of rapid screening was studied. Its main contents are as follows: 1. This paper reviews the status quo of illicit drugs in health food and Chinese patent medicine and the harm to consumers. The advantages of atmospheric direct ionization in the field of illicit drug detection were studied by comparing with the commonly used methods of drug detection. 2. Under the optimized experimental conditions, three phosphodiesterase 5 (PDE5) inhibitors, Vardenafil, sildenafil, and tadalafil, were rapidly detected by desorption corona beam ion source (DCBI) and ion trap mass spectrometry. The illegal additives in the samples were qualitatively identified by first stage mass spectrometry screening and confirmed by secondary mass spectrometry, and compared with the traditional high performance liquid chromatography-UV (HPLC-UV) detection method by semi-quantitative analysis of secondary characteristic fragment ions. The cleavage of three PDE5 inhibitors by secondary mass spectrometry was studied. Rapid analysis, less sample consumption, no use of other chemical reagents, no pollution detection. 3. Under the optimized experimental conditions, a DCBI-MS method was established for the rapid detection of 9 尾 2 receptor agonists. The illegal additives in the samples were qualitatively identified by first-order mass spectrometry screening and confirmed by second-order mass spectrometry, and semi-quantitative analysis was carried out by secondary characteristic fragment ions. The method is simple, rapid and sensitive without complicated pretreatment process. It can be used for rapid qualitative and semi-quantitative detection of 尾 _ 2-receptor agonists in cough and antiasthmatic drugs. 4. Taking anti-fatigue health food as the research object, the blank samples of different dosage forms (tablets, pills, capsules, mixture, liquor, syrup) were selected. The effect of substrate on the detection limits and semi-quantitative analysis of three PDE5 inhibitors, vardenafil, sildenafil, and tadalafil, was determined by blank plus standard method. The results of this study provide a reference for the determination of other objects in different dosage forms and excipients by DCBI-MS.
【学位授予单位】：湖南师范大学
【学位级别】：硕士
【学位授予年份】：2013
【分类号】：R155.5;R286;O657.63

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