【摘要】 将HZM-3大孔树脂磺化,动态法载银依次获得Ag+-1#、Ag+-2#、Ag+-3#、Ag+-4#、Ag+-5#共5种Ag+型配位树脂,通过它们对FK506的静态吸附与解吸实验优选出了Ag+-3#树脂,其吸附率为77%,解吸率为92%;Ag+-3#树脂与FK506形成络合物的稳定性受溶液极性的影响,在室温下的静态吸附曲线表明,其对FK506的配位吸附符合Langmuir单分子层吸附模型;Ag+-3#树脂配位层析分离FK506,当甲醇:乙酸乙酯(V/V)=50:50,上样量为8mg/m L,流速为1BV/h时,可在4.5倍柱体积内完成整个分离过程,合并不含类似物的收集液,浓缩后在HPLC上检测纯度为98.83%,收率为87.35%,无类似物FK520与2H-FK506检出;乙醇结晶最终产品的纯度达到99.6%以上,样品经过ICP-AES检测,在其检测限内未检测出Ag+。更多还原

【Abstract】 The five kinds of coordination resins containing Ag+, Ag+-1#, Ag+-2#, Ag+-3#, Ag+-4# and Ag+-5# were prepared by loading Ag+ on the sulfonated macroporous resins of HZM-3. The Ag+-3# resins were the best adsorbent for FK506 with adsorption efficiency of 77% and desorption efficiency of 92%. The stability of complex groups of Ag+ and FK506 was affected by the solution polarity, and the coordination adsorption data of FK506 at room temperature fitted Langmuir monolayer adsorption model. When ratio of methanol and acetic acid ethyl ester was 50:50(v:v), the adsorption capacity was 8mg/m L with flow rate of 1BV/h. The purification of FK506 by ligand chromatograph with the Ag+-3# resins could be finished within 4.5BV. Mixing and concentrating the elution of FK506 without analogues, the purity of FK506 was 98.83% and the recovery efficiency was 87.35%. The final purity of product was 99.6% or more by crystallization of ethanol, and Ag+ was not detected by ICP-AES.更多还原