HPLC法检测脱氢环氧甲基醌霉素中间体N-(2-乙酰氧基苯甲酰基)-2,5-二甲氧基苯胺及其杂质
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篇名: HPLC法检测脱氢环氧甲基醌霉素中间体N-(2-乙酰氧基苯甲酰基)-2,5-二甲氧基苯胺及其杂质
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摘要: 目的:建立检测脱氢环氧甲基醌霉素(DHMEQ)中间体N-(2-乙酰氧基苯甲酰基)-2,5-二甲氧基苯胺(MA)及其杂质的方法。方法:采用高效液相色谱法。色谱柱为Utimate AQ-C18,流动相为乙腈-0.05%磷酸(梯度洗脱),流速为1 ml/min,检测波长为 230 nm,柱温为30 ℃,进样量为10 μl。结果:MA与各杂质间以及各杂质之间的分离度均>1.5,理论板数以MA峰计≥5 000,保留时间约为41 min;MA、乙酰水杨酸甲酯、SM2、SM1、MA-6、水杨酸、MA-2的定量限(相当于MA样品的百分比)分别为0.04%、0.03%、0.01%、0.05%、0.05%、0.05%、0.05%,检测限(相当于MA样品的百分比)分别为0.01%、0.01%、0.004%、0.02%、0.02%、0.02%、0.02%;溶液稳定性及方法耐用性良好。结论:该方法专属性、检测限、耐用性均符合要求,可用于检测DHMEQ中间体MA及其杂质。
ABSTRACT: OBJECTIVE: To establish a HPLC method to determine DHMEQ intermediate N-(2-acetoxybenzoyl)-2,5-dimethoxyaniline(MA). METHODS: The column was Utimate AQ-C18 with mobile phase of acetonitrile-0.05% phosphoric acid (gradient elution) at a flow rate of 1 ml/min, detection wavelength was 230 nm, column temperature was 30℃, and the injection volume was 10 μl. RESULTS: The separation degrees of MA and the impurities were above 1.5, the number of theoretical plates (calculated with MA peaks) was no less than 5 000, retention time was about 41 min; the detection limits (the percentages of MA samples) of MA, methyl acetylsalicylate, SM2, SM1, MA-6, salicylic acid and MA-2 were 0.04%, 0.03%, 0.01%, 0.05%, 0.05%, 0.05% and 0.05%; detection limits (the percentage of MA samples) were 0.01%, 0.01%, 0.004%, 0.02%, 0.02%, 0.02% and 0.02%, respectively; the stability of solution and durability of method were good. CONCLUSIONS: The specificity, detection limit, and durability of the method are all in line with the requirements, which can be used for DHMEQ intermediate MA and its impurity.
期刊: 2016年第27卷第36期
作者: 胡克余,汪岩峰,余卫麟,马俊,邓双炳
AUTHORS: HU Keyu,WANG Yanfeng,YU Weilin,MA Jun,DENG Shuangbing
关键字: 脱氢环氧甲基醌霉素;中间体;N-(2-乙酰氧基苯甲酰基)-2,5-二甲氧基苯胺;杂质;高效液相色谱法
KEYWORDS: DHMEQ; Intermediate; N-(2-acetoxybenzoyl)-2,5-dimethoxyaniline; Impurity; HPLC
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