盐酸曲唑酮杂质对照品核磁共振定量方法的建立  

Establishment of a quantitative ~1H-NMR method for reference standards of trazodone hydrochloride impurity

作　　者：夏志鑫 冯玉飞[1] 张雅军[1] 王瑾[1] 肖新月[1] 吴先富[1] XIA Zhi-xin;FENG Yu-fei;ZHANG Ya-jun;WANG Jin;XIAO Xin-yue;WU Xian-fu(National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2019年第5期925-929,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立盐酸曲唑酮杂质对照品的核磁共振定量方法。方法:采用Bruker 500 MHz核磁共振谱仪,采集一维核磁共振氢谱,以对苯二甲酸二甲酯为内标物,扫描次数设为32次,采样时间为3.28 s,弛豫延迟时间(D1)的设置如下:盐酸曲唑酮杂质A和杂质F为20 s[以氘代二甲亚砜(DMSO-d_6)为溶剂],曲唑酮杂质B、杂质C、杂质D的D1为30 s(以氘代丙酮为溶剂),分别进行定量研究。结果:5个盐酸曲唑酮杂质对照品的qNMR结果与质量平衡法结果基本一致。结论:本文建立的qNMR方法简单快捷,准确度高,为盐酸曲唑酮的质量控制及其杂质对照品的定值提供了新的方法,同时,可作为质量平衡法定值结果的有力佐证。Objective:To establish a quantitative 1H-NMR method(qNMR) for reference standards of trazodone hydrochloride impurity.Methods:The 1D quantitative 1H-NMR spectra were collected at Bruker 500 MHz NMR spectrometer.Dimethyl terephthalate was used as the internal standard with the number for scan set at 32 and the acquisition time set at 3.28 s.The relaxation time delay(D1)was set at 20 s for impurities A and F of trazodone hydrochloride(DMSO-d6 used as the solvent) while 30 s for impurities B,C,D of trazodone hydrochloride(acetone-d6 used as the solvent) to carry out quantitative study.Results:The results of quantitative 1H-NMR method were basically consistent with those of mass balance method.Conclusion:The qNMR method is simple,rapid and accurate for the quality control of trazodone hydrochloride and quantitative determination of reference standards of trazodone hydrochloride impurity.Meanwhile,it provides a supportive evidence for the results of mass balance method.

关 键 词：盐酸曲唑酮杂质 核磁共振定量 对苯二甲酸二甲酯 质量平衡法 

分 类 号：R917[医药卫生—药物分析学]