新型质谱离子源在海洋医用食品快速检测中的应用研究

发布时间：2018-07-17 04:00

【摘要】：近年来,开发和生产具有抗肿瘤、抗癌、抗氧化、抗衰老等新型海洋医用食品逐渐成为备受关注的热点。海洋医用食品活性成分的分析测定多采用高效液相色谱法、液相色谱-质谱法及气相色谱-质谱法等。然而,这些方法通常需要复杂的预处理,操作过程繁琐、耗时长、污染样品,故该类技术无法满足海洋医用食品安全生产和监督过程中现场快速检测的需求。常压敞开式质谱离子源可对不需样品前处理的复杂基体样品进行快速分析检测。本课题拟基于载玻片作为样品承载的基底,开发新型液滴喷雾质谱离子源,构建新型液滴喷雾离子源质谱法(DSI-MS)。针对不同形态(固态、液态)的海洋医用食品,建立新型质谱液滴喷雾离子源-海洋医用食品活性成分快速检测方法;重点拓展其在海洋医用食品活性成分快速定性、定量中的应用研究。基于载玻片尖端作为样品的载体,构建新型液滴喷雾质谱离子源,建立新型液滴喷雾离子源质谱分析方法,优化相关参数,获得可靠、稳定、高效的离子化效率;以此为基础,进一步研究了液滴喷雾离子源离子化机理。以环磷腺苷葡胺注射液、三磷酸腺苷二钠注射液、注射用丁二磺酸腺苷蛋氨酸等医用注射液为研究对象,验证了新型液滴喷雾离子源质谱法应用于海洋医用食品有效成分的快速分析检测的可行性。基于新型液滴喷雾离子源质谱法,针对不同形态(固体、液体)的海洋医用食品,开发新型液滴喷雾离子源-海洋医用食品活性成分快速定性分析方法。以牛磺酸为研究对象,考察了电离模式、喷雾溶剂、空间位置和喷雾电压等参数对牛磺酸信号响应的影响,构建了固态和液态样品DSI-MS法。并以此为基础,对来自6个不同厂家的牛磺酸样品(3个固态样品、3个液态样品)进行了快速定性分析,6个样品中的活性成分均被快速、准确的检测到。基于新型液滴喷雾离子源质谱法,建立新型液滴喷雾离子源-海洋医用食品活性成分的快速定量分析方法。以源自海绵的阿糖腺苷的磷酸化产物单磷酸阿糖腺苷为模型,考察了电离模式、空间位置和喷雾电压等参数对单磷酸阿糖腺苷信号响应的影响。采用MS/MS等研究手段,以单磷酸阿糖腺苷的特征碎片离子(m/z211)为定量离子,建立线性回归方程y=96.44 x-389.08,线性相关系数R2为0.99,检出限LOD为1.7 ng/mL;加标浓度在5~50 ng/m L时回收率在91.7%~111.0%之间。在此基础上,对隆赋牌、大同牌和先强牌注射用单磷酸阿糖腺苷中的活性成分进行了定量分析,活性成分的含量分别为18.06、19.19和20.16 ng/mL,相对标准偏差(RSD)分别是6.6%、6.6%和6.9%。本文以载玻片尖端为样品载体,构建了新型液滴喷雾离子源质谱法,并针对海洋医用食品中活性成分的快速分析需求,建立了新型液滴喷雾离子源-海洋医用食品活性成分快速定性、定量分析方法,并成功用于不用形态的海洋医用食品快速定性、定量分析。该方法具有极强的耐基体干扰能力,还具有分析时间短、无污染、稳定、操作简单等优点。本课题为当前国内海洋医用食品活性成分快速分析检测提供了理论和实践依据,有助于海洋医用食品的安全生产和规范化生产,推动相关行业标准的建立,进一步促进海洋医用食品的开发与利用。
[Abstract]:In recent years, the development and production of new marine medical foods, such as anti-cancer, anti-cancer, antioxidation and anti-aging, have gradually become a hot spot. The analysis and determination of active components in marine medical foods are mostly high performance liquid chromatography, liquid chromatography mass spectrometry and gas chromatography-mass spectrometry. However, these methods usually require complex preconditioning. The operation process is tedious, time-consuming and pollute the sample. Therefore, this kind of technology can not meet the needs of rapid detection in the process of safety production and supervision of marine medical food. The atmospheric mass spectrometry ion source can be used for rapid analysis and analysis of complex matrix samples without the sample pretreatment. A new type of droplet spray ion source mass spectrometry (DSI-MS) was developed to develop a new type of droplet spray ionization mass spectrometry (DSI-MS). A new type of mass spectrometric droplet spray ion source was developed for rapid detection of active components in marine medical food. A new type of droplet spray mass spectrometry ion source is constructed based on the carrier of the tip of the slide plate, and a new type of droplet spray ion source mass spectrometry is set up to optimize the related parameters to obtain reliable, stable and efficient ionization efficiency. Based on this, the ionization source ionization of droplet spray is further studied. Mechanism. With Meglumine Adenosine Cyclophosphate Injection, Adenosine Disodium Triphosphate Injection, injection of adenosylmethionine butyl two and other medical injections as the research object, the feasibility of rapid analysis and detection of effective components of marine medical food by a new droplet spray ion source mass spectrometry was verified. For the marine medical food with different forms (solid and liquid), a rapid qualitative analysis method for the active components of marine medical food was developed by a new type of droplet spray ion source. The effects of the parameters of taurine on the response of the sulfonic acid signal, such as ionization mode, spray solvent, space position and spray voltage, were investigated, and the solid and liquid were constructed. Based on the DSI-MS method, a rapid qualitative analysis of taurine samples (3 solid samples and 3 liquid samples) from 6 different manufacturers was carried out. The active components of the 6 samples were quickly and accurately detected. Based on the new droplet spray ion source mass spectrometry, a new type of droplet spray ion source - Marine medical food was established A rapid quantitative method for analysis of active components. The effects of ionization mode, space position and spray voltage on the response of adenosine monophosphate signal were investigated with the model of arabinosine monophosphate monophosphate monophosphate from spongy adenosine adenosine as a model. The characteristic fragment ion (m/z) of adenosine monophosphate, such as MS/MS, was used. 211) for the quantitative ion, the linear regression equation y=96.44 x-389.08 is established, the linear correlation coefficient R2 is 0.99, the detection limit is 1.7 ng/mL, and the recovery rate of the standard concentration at 5~50 ng/m L is between 91.7%~111.0%. On this basis, the active components in the long Fu brand, Datong brand and the first strong brand Vidarabine Monophosphate for Injection are quantitatively analyzed. The content of the sex components is 18.06,19.19 and 20.16 ng/mL respectively, and the relative standard deviation (RSD) is 6.6%, 6.6% and 6.9%. respectively. In this paper, a new type of droplet spray ion source mass spectrometry is constructed in this paper, and a new type of droplet spray ion source, marine medicine, is established for the rapid analysis of the active components in marine medical food. The fast qualitative and quantitative analysis method of food active ingredients has been successfully applied to the rapid qualitative and quantitative analysis of the non morphologic marine medical food. The method has the advantages of very strong resistance to matrix interference, short analysis time, no pollution, stability, simple operation and so on. This topic is a fast active ingredient in the current domestic marine medical food. The analysis and testing provide theoretical and practical basis, which will help the safety production and standardized production of marine medical food, promote the establishment of related industry standards, and further promote the development and utilization of marine medical food.
【学位授予单位】：哈尔滨工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TS218;O657.63

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