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建立了测定无对照品的新型二醇酯类内给电子体(6#酯、7#酯)纯度的核磁共振氢谱内标测定法。实验以氘代氯仿为溶剂,以苯甲酸甲酯标准物质为内标,设定合适的采样时间和延迟时间,选取适合的内标峰和样品定量峰,方法测定结果的相对标准偏差分别为0.31%和0.37%(n=6),且呈现良好的线性关系。样品经测量后的纯度平均值分别为98.6%和98.4%,与HPLC法测定结果符合。在没有标准对照品的情况下,核磁共振氢谱内标法可用于该二醇酯类内给电子体的纯度测定。
The internal standard method of 1H NMR was established for the determination of purity of new diol ester internal donors (6 # ester, 7 # ester) without reference substance. The experiment uses deuterated chloroform as solvent and methyl benzoate as internal standard, sets appropriate sampling time and delay time, selects suitable internal standard peak and sample quantitative peak, and the relative standard deviations of the method are 0.31 % And 0.37% (n = 6), and showed a good linear relationship. The average purity of the samples after measurement was 98.6% and 98.4%, respectively, which was in good agreement with the HPLC method. In the absence of a standard reference substance, the internal standard method of 1H NMR can be used for the purity determination of the electron donor in the diol ester.