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A simple and specific quantitative method for determination of dictamnine in Dictamni Cortex by ~1H NMR spectroscopy

机译:〜1H NMR光谱法测定麦草皮中香茅碱的简单,定量方法

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摘要

Dictamni Cortex (Baixianpi) is a commonly used medicinal herb in traditional Chinese medicines (TCMs), possessing various bioactivities. Quinoline alkaloids are regarded as one of the main active components in this herb. In the present study, a more convenient, specific and accurate analytical method using ~1H NMR has been developed for the quantitative determination of dictamnine, one of the main active quinoline alkaloids in Dictamni Cortex. In a less crowded region δ 8.0-8.5, the signal of H-5 of dictamnine was well separated from other signals in chloroform-di. The quantity of dictamnine was calculated by means of the integral value of H-5 of dictamnine to that of the known amount of internal standard, pyrazine. This assay was precise and reproducible, with RSDs less than 3%. The recovery results of dictamnine were observed between 92.10 and 108.10% and the limit of detection (LOD) and limit of quantitation (LOQ) were 3.3 ug ml~(-1) and 13.2 ug ml~(-1), respectively. This newly developed method was proven to be highly accurate, precise and robust, for the determination of dictamnine in Dictamni Cortex. The results obtained from ~1H NMR method were also compared with those from conventional HPLC method, and no remarkable difference was found between these two methods.
机译:Dictamni Cortex(百仙皮)是中药(TCM)中常用的草药,具有多种生物活性。喹啉生物碱被认为是该草药的主要活性成分之一。在本研究中,已开发出一种更方便,更具体,更准确的分析方法,即使用〜1H NMR定量测定dictamnine,Dictamniine是Dictamni Cortex中的主要活性喹啉生物碱之一。在较不拥挤的区域δ8.0-8.5中,十氢丁胺的H-5信号与氯仿-di中的其他信号完全分开。胺的含量是通过胺的H-5相对于内标物吡嗪的已知量的积分值算出的。此测定法精确且可重复,RSD小于3%。烟酰胺的回收率在92.10%至108.10%之间,检出限(LOD)和定量限(LOQ)分别为3.3 ug ml〜(-1)和13.2 ug ml〜(-1)。事实证明,这种新开发的方法非常准确,精确且稳定,可用于测定Dictamni皮层中的吗啡宁。还将〜1H NMR方法获得的结果与常规HPLC方法获得的结果进行了比较,发现这两种方法之间没有显着差异。

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