摘要
目的研究发酵液中手性扁桃酸的分离纯化工艺。方法采用pH值电位滴定法测定扁桃酸的离解常数,采用高效液相色谱法考察扁桃酸在不同溶剂中的溶解度曲线,采用动态吸附和动态解吸法进行离子交换分离工艺的筛选。结果扁桃酸的离解常数pK_a值为5.28。扁桃酸在水和苯中的溶解度曲线可分别表示为:S=38.756 e^(0.0354T)和S=0.2746 e^(0.0649T);扁桃酸在水和苯中的溶解度差值曲线可分别表示为:△S/S_1=0.1196 T-2.712和△S/S_1=0.3688 e^(0.0723T)。采用711树脂从发酵液中离子交换分离扁桃酸时,最适动态吸附条件为上柱液扁桃酸浓度100 mmol/L、流速0.5 Bv/h、pH值6.4~7.2、最适动态解吸条件为2.0%NaOH、解吸流速0.5 BV/h。扁桃酸纯化工艺条件为70℃热苯萃取和10℃冷却结晶。结论采用本分离纯化工艺,发酵液中手性扁桃酸的提取率为87.8%,纯度≥98%。
OBJECTIVE To study a new method for the separation and purification of chiral drugs mandelic acid from ferment broth.METHODS The ionization constant of mandelic acid was mensurated by pH potentiometer titration.The solubility curves of mandelic acid in different solvent were determined by HPLC.The separation technics of mandelic acid by ion exchange technology was chosed by dynamic adsorption and dynamic desorption.RESULTS The ionization constant pK_a of mandelic acid was 5.28.the solubility of mandelic acid in water and benzene could be respectively denoted with S = 38.756 e^(0.0354T) and S = 0.2746 e^(0.0649T),and the difference of solubility of mandelic acid in water and benzene could be respectively denoted with △S/S_1 = 0.1196 T- 2.712 and △S/S_1 = 0.3688 e^(0.0723T).While mandelic acid separated from ferment broth at 711 anion exchange resin,the optimum dynamic adsorption condition was 100 mmol/L mandelic acid concentration、6.4~7.2 pH value and 0.5 Bv/h velocity of flow,the optimum dynamic desorption condition was 2%NaOH concentration and 0.5 Bv/h velocity of flow.The purification technics was 70℃ benzene extraction and 10℃ refrigeration crystal.CONCLUSION 87.8%mandelic acid more than 98%purity could be separated from ferment broth a by this separation and purification technics.
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2005年第z1期624-628,共5页
Chinese Journal of Modern Applied Pharmacy
基金
福建省科技厅重点(2003H023)
福建省计委(闽计46号)
福州大学SRTP(03166)资助项目
关键词
手性药物
扁桃酸
发酵液
分离
纯化
chiral drugs
mandelic acid
ferment broth
separation
purification
