通过实验室练习向生物医学实验室科学家介绍核磁共振用1H-NMR台式仪器合成、结构测定及定量阿司匹林

Marit Kristin Leiren, S. Steinkopf
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引用次数: 0

摘要

在这次化学教育研究中,NMR被引入到一组3名非化学背景的学生中。采用台式核磁共振仪采集了1h -NMR光谱。利用1h - nmr谱监测ASA的合成及产物纯度。产品的光谱证实了它的形成,而原油和最终产品的光谱让学生们观察到产品再结晶时杂质的消除。此外,通过质子共振的积分,最终产物的光谱被用来量化产率。利用质子共振积分来计算ASA的产率,据我们所知,在本科生实验中没有其他地方描述过。本文报道了氢核磁共振谱的合成、记录和处理以及产率的计算过程。这个程序可以由本科生或高中生实施,也可能对那些想在化学课程早期引入核磁共振波谱的教师有用。通过这样的练习,学生们获得了使用先进技术的经验,这些技术将来可能会在医院实验室中普遍使用。此外,在化学课程中尽早引入一种要求最高、最先进的化学方法,有助于促进化学事业的发展。
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Introducing NMR to Biomedical Laboratory Scientists through a Laboratory Exercise; Synthesis, Structure Determination and Quantization of Aspirin by Employing an 1H-NMR Bench Top Instrument
In this chemical education research study, NMR was introduced to a group of 3 students with minor chemistry background. A bench top NMR instrument was used to acquire the 1 H-NMR spectra. The 1 H-NMR spectra were used to monitor the synthesis of ASA and product purity. The spectrum of the product confirmed its formation, and the spectra of crude and final product allowed the students to observe the elimination of impurities upon recrystallization of the product. Further, the spectrum of the final product was used to quantify the yield through integration of the proton resonances. The use of integrals of the proton resonances for calculation of the yield of ASA is to our knowledge not described elsewhere in undergraduate experiments. A procedure for the synthesis, recording and processing of 1 H-NMR spectra, as well as calculation of the yield is reported. This procedure can be implemented by undergraduate or by high school students and might as well be useful for instructors who wants to introduce NMR spectroscopy early in the curriculum of Chemistry. By including an exercise like this, the students get hands on experience to employ advanced technology that might be commonly used in the future, also in Hospital laboratories. Furthermore, it is useful to introduce one of the most demanding and advanced methods in chemistry as early as possible in the curriculum in Chemistry to promote the chemistry career.
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