核磁共振定量法测定盐酸莫西沙星的含量

Determination of moxifloxacin hydrochloride by quantitativenuclear magnetic resonance

采用氢核磁共振定量法和氟核磁共振定量法测定盐酸莫西沙星的含量。氢核磁共振定量法以盐酸莫西沙星δ=8.66处为定量峰,3,5-二甲基吡唑δ=5.74处为内标峰,对应测定条件为恒温25℃、脉冲宽度14.8 s、扫描次数16次、采样时间4 s、弛豫延迟时间15 s。氟核磁共振定量图谱在恒温25℃、谱宽12500 Hz、中心频率-43662.7 Hz的条件下采集,并以三氟乙酸作为内标。结果表明:使用氢核磁共振定量法和氟核磁共振定量法测定出盐酸莫西沙星的含量与使用质量平衡法的结果基本一致。由此可知,核磁共振定量法可用于盐酸莫西沙星含量的测定,并且具有快速、准确以及操作简单等优势。

A novel quantitative proton nuclear magnetic resonance(qHNMR)and quantitative fluorine nuclear magnetic resonance(qFNMR)method was used for the determination of moxifloxacin hydrochloride.The 1 H NMR spectra were collected withδ=8.66 of moxifloxacin hydrochloride as quantitative peaks andδ=5.74 of 3,5-dimethylpyrazole as internal standard peak,and the corresponding condition were 298 K,14.8 s pulse width,16 scanning times,4 s sampling time and 15 s relaxation delay.The 19 F NMR spectra were obtained at 298 K by using 12500 Hz spectral width and-43662.7 Hz transmitter frequency offset,and trifluoroacetic acid was employed as internal standard.The experimental results show that the content of moxifloxacin hydrochloride determined by qHNMR and qFNMR methods was basically consistent with that of the mass balance method.Therefore,quantitative nuclear magnetic resonance can be used for the quantitative determination of moxifloxacin hydrochloride,and has the advantages of fast,accurate,and simple operation compared to other methods.