核磁共振内标法测定波生坦的含量

Quantitative determination of bosentan by proton nuclear magnetic resonance with internal standard method

建立1H NMR核磁共振定量法(简称QNMR)测定波生坦的含量。采用Bruker AVANCEⅡ400型核磁共振谱仪,以对苯二甲酸二甲酯为内标,氘代氯仿为溶剂,zg30脉冲序列获取1H NMR谱,测定波生坦的含量,并与采用质量平衡法计算含量的结果进行比较。采用核磁定量法与质量平衡法测定本品含量分别为96.25%与96.58%。本文建立的核磁定量的方法准确、快速,为该品种的质量控制和首批对照品的标定提供了新的方法,并为质量平衡法定值提供有力的佐证。

The study aims to establish a quantitative nuclear magnetic resonance （QNMR） method for the determination of the absolute content of bosentan. Proton nuclear magnetic resonance spectroscopy [ 1H NMR] spectra were obtained in CDC13 with the internal standard dimethyl terephthalate and zg30 pulse sequence by using a Bruker AVANCE II 400 spectrometer. The content of bosentan is determined with QNMR in comparison with the result obtained by mass balance method. The result is 96.25% by QNMR and 96.54% by mass balance method. A rapid and accurate QNMR method has been established for the quantitative determination of the absolute content of bosentan. The study provides a new way for the quality control and calibration of a new reference standard material, it could be the complementary with the mass balance method for the assay of standard reference.