摘要
目的采用核磁共振定量法(QNMR)测定阿戈美拉汀的绝对含量。方法采用AvanceⅢ400型核磁共振谱仪,zg30脉冲序列在25℃下获取1HNMR谱。以对苯二酚为内标,测定了阿戈美拉汀Ⅱ型晶体含量。结果分别以阿戈美拉汀中的峰δ1.89、3.15、3.40、3.97、7.19、7.27、7.33、7.66、7.70、7.81、8.17及对苯二酚的单峰δ6.63作为定量峰,含量分别为99.43%、99.25%、99.58%、99.33%、99.40%、99.60%、99.50%、99.30%、99.60%、99.70%、98.40%。采用不同的峰定量结果的RSD=0.35%(n=11);剔除以酰胺活性氢定量的结果,RSD=0.15%(n=10);重复性试验的RSD=0.25%(n=5)。结论采用QNMR能准确快捷地测定阿戈美拉汀的绝对含量,并定性与定量其中的未知杂质,是对标准物质绝对含量测定的一种补充。
OBJECTIVE To establish a quantitative nuclear magnetic resonance（QNMR） method for the determination of the absolute content of Agomelatine. METHOD Proton nuclear magnetic resonance spectroscopy（^1HNMR） spectra were obtained in DMSO - d6 with zg30 pulse sequence by using an Avance Ⅲ400 spectrometer at 25℃ and p - dihydroxybenzene was used as interual standard to quantify the absolute content of Agometaline. RESULTS The analysis of 1HNMR spectrum of Agomelatine mixed with p - dihydroxybenzene as internal standard in DMSO - d6 revealed that the integration of signals at δ1.89,3.15,3.40,3.97,7.19,7.27, 7.33,7.66,7.70,7.81 or 8.17 of Agomelatine and δ6.63 of p - dihydroxybenzene could used for quantification respectively and the results of the contents of Agomelatine were 99.43% ,99.25% ,99.58% ,99.33% ,99.40% ,99.60% ,99.50% ,99.30% ,99.60%, 99.70% and 98.40%. The RSD of contents data was 0.35% （ n = 11 ） with the amide proton signal method included and 0.15% （ n = 10） without it,respectively. The precision RSD of repetitive tests was 0.25% （ n =5 ）. CONCLUSION QNMR can be used for the quantitative determination of the absolute content of Agomelatine rapidly with high precision and quatitative and quantitative detected unknown impurity. It is a good supplementary method for determing the absolute content of the reference standard.
出处
《华西药学杂志》
CAS
CSCD
北大核心
2014年第3期306-307,共2页
West China Journal of Pharmaceutical Sciences
关键词
抗抑郁药
阿戈美拉汀
核磁共振定量
标准物质
绝对含量
定量分析
对苯二酚内标
Antidepressant
Agomelatine
Quantitative nuclear magnetic resonance （QNMR）
Standard substance
Absolute concentrations
Quantitative analysis
p - dihydroxybenzene internal standard
