核磁共振和液相色谱-质谱法对苯丙哌林未知杂质的结构分析

发布时间：2018-01-19 00:17

本文关键词： 苯丙哌林有关物质核磁共振波谱液相色谱质谱联用波谱归属杂质结构确证　出处：《药物分析杂志》2017年11期 　论文类型：期刊论文

【摘要】：目的:建立利用仪器分析苯丙哌林未知杂质化学结构的方法,并对2个未知杂质进行结构确证。方法:采用Inertsil ODS-3(4.6μm,2.1 mm×150 mm)色谱柱,以甲醇-0.01 mol·L~(-1)醋酸铵缓冲液(取醋酸铵0.77 g,加水800 m L溶解,用冰醋酸调节p H至3.3,用水稀释至1 000 m L)(65∶35)为流动相,流速0.25 m L·min~(-1),检测波长270 nm。用HPLC-MS/MS分析2个未知杂质,使用制备液相进行分离纯化,通过核磁共振(~1H-NMR、~(13)C-NMR、HMBC、HSQC、DEPT135、H-H COSY)技术,对苯丙哌林及其未知杂质进行结构确证。结果:首次发现并确定苯丙哌林2个未知杂质的结构,分别为1-[2-(2-苯甲酰基苯氧基)-1-甲基乙基]哌啶和1-[2-(2-苄基-6-氯苯氧基)-1-甲基乙基]哌啶。结论:该方法可为苯丙哌林的质量控制提供依据。
[Abstract]:Objective: to establish a method for analyzing the chemical structure of unknown impurity in benoperazine by means of instrument, and to confirm the structure of two unknown impurity. Methods: Inertsil ODS-3(4.6 渭 m was used to determine the chemical structure of the unknown impurity. The chromatographic column was 2. 1 mm 脳 150 mm and dissolved in methanol-0.01 mol 路L ~ (-1) ammonium acetate buffer solution (ammonium acetate 0.77 g, water 800 mL). The mobile phase was adjusted with glacial acetic acid to 3.3, diluted to 1 000 mL / 35 with a flow rate of 0.25 mL 路min ~ (-1). The detection wavelength was 270nmm. two unknown impurities were analyzed by HPLC-MS/MS and separated and purified by liquid phase. HMBCU HSQCU DEPT135 H-H COSYY technology. Results: for the first time, the structure of two unknown impurity of benoperazine was found and determined, and the structure of the two unknown impurity was 1-. [2-BENZOXYLPHENOXYLPHEXYLPHENOXYL] piperidine and 1-METHYLETHYL. [Conclusion: this method can provide the basis for the quality control of benoperazine.
【作者单位】：黑龙江省食品药品检验检测所;
【分类号】：R927.1
【正文快照】： 第一作者Tel:13936401209;E-mail:limsn@163.com苯丙哌林(benproperine)为非成瘾性镇咳药。能抑制咳嗽中枢,也能抑制肺及胸膜牵张感受器引起的肺-迷走神经反射,且有平滑肌解痉作用,是中枢性和末梢性双重作用的强效镇咳药,其镇咳作用比可待因强[1-3]。该药目前在我国使用广泛,

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