摘要
[目的]工业中要通过多次重结晶提纯阿维菌素才能得到纯度较高的产品,生产成本大。提出阿维菌素提纯的溶析结晶工艺,减少操作成本。[方法]通过高效液相色谱法和显微镜观察法考察不同溶剂和溶析剂对产品纯度、杂质含量以及产品晶习的影响。[结果]通过1次溶析结晶产品B1纯度可以达到95%以上。得到的产品一般是粒状或者棱柱状。[结论]乙酸乙酯为溶剂、乙醇为溶析剂得到的产品B1纯度最高,而丙酮作溶剂、水为溶析剂对某些杂质有更好的去除效果。溶析结晶得到的产品一般是粒状或者棱柱状,相对冷却结晶得到的针状晶体有利于后续过滤、洗涤、干燥等过程。
[Aims] Three or more recrystallizations are needed to get the final products of avermetins, leading to high cost in industry. Solvent-out crystallization of avermectins was proposed to reduce the cost. [Methods] The effect of solvent/anti-solvent on the product purity, impurity content and crystal habits was investigated by high performance liquid chromatography and microscope. [Results] B, Content of avermectins product reached 95% by one step solvent-out crystallization, the products are generally prismatic or granular. [Conclusions] The purity of products produced in ethyl acetate as solvent and ethanol as anti-solvent was the highest. Acetone as solvent and water as anti-solvent might be more effective in removing certain impurities than other solvent/anti-solvent groups. Compared with the needle-shaped crystal obtained by cooling crystallization in ethanol, the products produced through solvent-out crystallization are generally prismatic or granular, which is helpful for filtration, washing and drying in industrial crystallization of avermectins.
出处
《农药》
CAS
北大核心
2011年第9期638-640,共3页
Agrochemicals
基金
天津市自然科学基金(09JCZDJC2011
10JCYBJC14200)
国家自然科学基金(30900540)
关键词
阿维菌素
溶析结晶
纯度
晶习
avermectins
solvent-out crystallization
purity
crystal habit
