Surfactant-free air bubble flotation?coagulation for the rapid purification of chloroquine
Surfactant-free air bubble flotation?coagulation for the rapid purification of chloroquine
复制标题
无表面活性剂气泡浮选混凝快速纯化氯喹
DOI：
10.1007/s44211-022-00196-2
复制
发表时间：
2022
影响因子：
1.6
通讯作者：
Saitoh Tohru
中科院分区：
文献类型：
--
作者：
Kodama Koki;Saitoh Tohru
设计了一种简单、快速的无表面活性剂气泡浮选-混凝分离方法，用于氯喹粗品的提纯。使用具有烧结玻璃过滤器（用于柱色谱法）的开放玻璃柱作为浮选容器。通过将粗CQ倒入含有0.1%（v/v）的2-丙醇的水溶液中，随后通过玻璃过滤器进料空气以产生气泡来进行浮选。在pH值为12时，CQ在气泡浮选开始后90 s内富集到水面暂时产生的泡沫中，形成混凝物。另一方面，反应物; 4，7-二氯喹啉和4-氨基-1-二乙基氨基戊烷，以及产生的杂质保留在本体水溶液中。动态表面张力的测定结果表明，CQ分子选择性地吸附在空气-水界面上，而混凝剂在界面上的吸附更强烈。分子动力学模拟的计算结果也再现了CQ分子在空气-水界面上的吸附和凝聚过程。通过抽吸从水面收集凝聚物，然后倒入另一个浮选容器中进行重复分离。包括气泡浮选和通过抽吸收集的各个分离过程所需的时间在5分钟内。经3次分离，得到纯度> 99.0%的CQ，收率为72 ± 8%。反应物和其他杂质的量减少到无法检测的水平。图形摘要
A simple and rapid separation method based on surfactant-free air bubble flotation and coagulation was designed for the purification of chloroquine (CQ) from its crude product. An open glass column having a sintered glass filter (for column chromatography) was used as a flotation vessel. The flotation was conducted by pouring the crude CQ into the aqueous solution containing 0.1% (v/v) of 2-propanol followed by feeding air through the glass filter to generate air bubbles. At pH 12, CQ was enriched into the foam temporary generating on the surface of water to form the coagulates within 90 s after the start of the air bubble flotation. On the other hand, reactants; 4,7-dichloroquinoline and 4-amino-1-diethylaminopentane, as well as generated impurities remained in the bulk aqueous solution. The result of dynamic surface tension measurement indicated that CQ molecules selectively adsorbed on the air–water interface and the coagulates more strongly adsorbed the interface. Adsorption and coagulation of CQ molecules on the air–water interface were also reproduced in the calculation results of a molecular dynamic simulation. The coagulates were collected from the surface of water by suction and then poured into another flotation vessel for conducting repeated separation. The time required for the respective separation process including air bubble flotation and collection by suction was within 5 min. After three-times separation, highly purified (> 99.0%) CQ was obtained with a yield of 72 ± 8%. The amounts of reactants and other impurities reduced into undetectable levels.Graphical abstract