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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+。
The HZM-3 macroporous resin was sulfonated and supported by dynamic method. Five kinds of Ag + type coordination resin were obtained by Ag + -1 #, Ag + -2 #, Ag + -3 #, Ag + -4 # and Ag + -5 # Their adsorption and desorption experiments FK506 preferred Ag + -3 # resin, the adsorption rate was 77%, the desorption rate was 92%; Ag + -3 # resin and FK506 complexes formed by the stability of the solution polarity , The static adsorption curve at room temperature showed that the adsorption of FK506 was in accordance with the Langmuir monolayer adsorption model. The FK506 was separated by Ag + -3 # resin coordination chromatography. When methanol: ethyl acetate (V / V) = 50:50, the sample volume of 8mg / m L, the flow rate of 1BV / h, the complete separation can be completed within 4.5 times the column volume, the merger without the collection of analogs, concentrated after HPLC purity of 98.83 %, The yield was 87.35%, no analog FK520 and 2H-FK506 detected; ethanol purity of the final product of more than 99.6%, ICP-AES samples detected in the detection limit was not detected Ag +.