核磁共振定量法测定利培酮含量  

Determination of Risperidone by Quantitative Nuclear Magnetic Resonance

作　　者：郭留城[1] 郝海军[2] 杜利月[1] GUO Liu-cheng;HAO Hai-jun;DU Li-yue(Department of Pharmacy,Luohe Medical College,Luohe 462000,China;Instrumental Analysis ＆ ResearchCenter,Shanghai Institute of Pharmaceutical Industry,Shanghai 201203,China)

机构地区：[1]漯河医学高等专科学校药学系,河南漯河462000 [2]上海医药工业研究院分析测试中心,上海201203

出　　处：《分析测试学报》2018年第4期492-495,共4页Journal of Instrumental Analysis

基　　金：2017年度河南省高等学校青年骨干教师培养计划(2017GGJS286)

摘　　要：采用氢核磁共振定量法和氟核磁共振定量法测定利培酮含量。氢核磁共振定量法以利培酮δ7.29~7.35处质子峰为定量峰,马来酸δ6.02处为内标峰,在恒温300 K,采样时间4.0 s,弛豫延迟时间15 s,扫描次数为32次条件下采集氢谱。氟核磁共振定量法以4-溴-2-氟-乙酰苯胺为内标,在恒温300 K,谱宽12 500.0 Hz,中心频率-43 662.7 Hz下采集氟谱。测试结果显示,利培酮氢核磁共振定量法和氟核磁共振定量法的含量测定结果基本与质量平衡法的结果一致。因此,核磁共振法可用于利培酮绝对含量的测定,具有快速、简单、准确的优势。Proton nuclear magnetic resonance （qHNMR ） and fluorine nuclear magnetic resonance （qFNMR ） were employed to determine the content of risperidone.The 1H NMR spectra were collected at 300 K within 4.0 s acquisition time,15 s relaxation delay and 32 scanning times.Proton signal peaks at δ 7.29-7.35 of risperidone and δ 6.02 of maleic acid were served as quantitative peaks.The 19 F NMR spectra were obtained at 300 K by using 12 500.0 Hz spectral width and -43 662.7 Hz transmitter frequency offset （O1 ）.4-bromo-2-fluorine acetanilide was employed as the internal standard.The results of qHNMR and qFNMR were generally consistent with that of the mass balance method.Therefore,quantitative nuclear magnetic resonance could be used for the quantitative determination of risperidone.

关 键 词：利培酮 核磁 氢核磁共振定量法 氟核磁共振定量法 

分 类 号：O482.532[理学—固体物理] TQ460.72[理学—物理]