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米托蒽醌的合成及质量评价
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| 篇名： | 米托蒽醌的合成及质量评价 |
| TITLE： | |
| 摘要： | 目的：合成米托蒽醌并对其进行质量评价。方法：采用1，4，5，8-四羟基蒽醌为原料，氩气保护下，50 ℃水浴条件中与N-（2-羟乙基）乙二胺反应2 h，经干空气缓慢氧化4 h后制得米托蒽醌粗品，粗品结晶以乙醇-正己烷（4 ∶ 1，V/V）混合液热溶冷却过夜析晶后，经乙醇-正己烷混合液多次洗涤制得米托蒽醌精品。考察精品（4批）的熔点、水溶液pH、紫外-可见吸收光谱、红外结构特征、干燥失重（失水率）和临界相对湿度（CRH）等，采用高效液相色谱（HPLC）法测定其中米托蒽醌的含量。结果：成功合成米托蒽醌，合成产率为34.3％，熔点为159.1～163.6 ℃，水溶液显碱性（pH为7.63～9.54），235～245 nm波长范围内出现紫外最大吸收峰，590～600 nm波长范围内出现可见光最大吸收峰，红外特征与《药品红外光谱集》（2015年版）米托蒽醌项下描述一致，失水率为－0.83％～2.36％，CRH为54.7％，HPLC法测得平均含量为78.1％（n＝4）。结论：本文通过温和、无毒无害的试验条件成功合成米托蒽醌，合成步骤简单、成本低廉、产率高，合成产品质量符合相关要求。 |
| ABSTRACT： | OBJECTIVE： To synthetize the synthesis of mitoxantrone and evaluate its quality. METHODS： Crude product of mitoxantrone was prepared by slow oxidation of 1，4，5，8-tetrahydro-anthraquinone with N-（2-hydroxyethyl） ethylenediamine in water bath at 50 ℃ for 2 h under argon protection and in dry air for 4 h. The crude product was crystallized by ethanol-n-hexane （4 ∶ 1，V/V） mixture solution， which was cooled overnight and then washed by ethanol-n-hexane mixture for many times. The melting range， pH value of solution， ultraviolet-visible absorption spectrum， infrared structural characteristics， drying weight loss （water loss rate） and critical relative humidity （CRH） of the purified products （4 batches） were investigated. HPLC method was used to determine the contents of mitoxantrone. RESULTS： The mitoxantrone was prepared successfully， and synthetic yield of mitoxantrone was 34.3％； the melting point ranged from 159.1-163.6 ℃. The aqueous solution was alkaline （pH 7.63-9.54）； there was a maximum ultraviolet absorption peak at 235-245 nm； there was a maximum absorption peak of visible light at 590-600 nm； the infrared characteristics were consistent with those described of mitoxantrone in the 2015 edition of the Infrared Spectrum Collection of Drugs； water loss rate were －0.83％-2.36％； CRH value was 54.7％， and the average content of the product was 78.1％（n＝4） by HPLC method. CONCLUSIONS： The mitoxantrone is synthesized under mild， non-toxic and harmless experiment conditions. The synthesis step is simple， the cost is low and the yield is high. The quality of products meets the quality requirements. |
| 期刊： | 2019年第30卷第13期 |
| 作者： | 王明明，蔡锦源，刘京，顾浦中，侍慧慧，张艳军 |
| AUTHORS： | WANG Mingming，CAI Jinyuan，LIU Jing，GU Puzhong，SHI Huihui，ZHANG Yanjun |
| 关键字： | 米托蒽醌；合成；质量评价；高效液相色谱法 |
| KEYWORDS： | Mitoxantrone； Synthesis； Quality evaluation； HPLC |
| 阅读数： | 894 次 |
| 本月下载数： | 14 次 |
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