目的: 采用氢核磁共振定量法测定连翘苷的绝对含量。方法: 以DMSO-d6-氘代三氯甲烷(1∶1)作为溶剂,以苯二甲酸二甲酯(DMT)为内标,通过比较DMT化学位移δ 3.92内标峰的峰面积和连翘苷化学位移δ 7.06定量峰的峰面积,采用氢核磁共振定量法测定连翘苷的绝对含量。结果: 该方法精密度小于0.031%,线性相关系数为0.999 9,采用此实验中的核磁定量法测得本实验室制备该样品中连翘苷的含量为93.01%~93.32%。结论: 本文建立的核磁定量法操作简单,快速准确,为连翘苷的含量测定提供了新的方法。
Objective: To determine the absolute content of phillyrin by 1H nuclear magnetic resonance quantitative method(qNMR). Methods: DMSO-d6 and deuterated chloroform (1∶1) were used as the solvent and dimethyl terephthalate (DMT) was used as the internal standard. Through comparing the internal standard peak area of DMT at δ 3.92 and the quantitative peak area of phillyrin at δ 7.06, the absolute content of phillyrin was determined by qNMR. Results: The precision of this method was less than 0.031%, and the linear correlation coefficient was 0.999 9. The content of phillyrinin the sample prepared in our laboratory was within 93.01%-93.32% by qNMR. Conclusion: The NMR quantitative method established in this paper is simple, rapid and accurate, and provides a new method for the determination of phillyrin.
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