1-(α-萘甲基)-2甲基-6,7-二甲氧基-1,2,3,4-四氢异喹啉盐酸盐的HPLC手性拆分法及半制备

1-(α-Naphthylmethy)-2-methyl-6,7-dimethoxy-1,2,3,4-tetrahydroisoquinolinehydrochloride (code No, 86040)is a new kind of calcium antagonist. It has(+)and(一)enantiomers.Accordingly .the resolution and quantification of these two enantiomers have received agreat deal of attention,In this report the application of direct HPLC separation and semipreparation tothe determination of the enantiomeric composition of the new drug are described. All analysis andsemipreparation were performed with 25 cm×4. 6 mm i.d, 25 cm×8 mm i,d.and 30 cm×8 mmi.d. stainless steel column packed with a chiral β-cycledextrin bonded phase. Detection wavelengthwas 284 nm, The optimal composition of the mobile phase was EtOH─pH 4.0 phosphate buffer(35:65) at flow rate of 0. 3 ml·min^-1 for analysis and l.0 ml·min^-1 for semipreparation. Theseparation factor of the enantiomers was l.25. Purity of the semipreparation was 8l.4%,Quantityof semipreparation was 1 mg. This procedure was simple ,rapid and gave good resolution,The effectsof the composition of mobile phase, pH value, flow rate and column temperature on the resolution hadbeen sudied.     

1－（α－萘甲基）－2甲基－6，7－二甲氧基－1，2，3，4－四氢异喹啉盐酸盐的HPLC手性拆分法及半制备

１－（α－萘甲基）－２甲基－６，７－二甲氧基－１，２，３，４－四氢异喹啉盐酸盐的ＨＰＬＣ手性拆分法及半制备王义明，罗国安，彭健斌，詹少卿，刘子列，林炳承（清华大学化学系，北京１０００８４）目前已知药物中约有３０～４０％是手性对映体（ｅｎａｎｔｉｏｍｅ...     

高效液相色谱法测定磺丁基-β-环糊精中的β-环糊精残留含量

目的:建立磺丁基-β-环糊精中有关物质β-环糊精检测及含量测定的高效液相色谱分析。方法:采用Waters XTerraMs-C18(4.6 mm×250 mm,5μm)柱;流动相:甲醇-水(8∶92);检测器:示差折光率检测器;流速:0.8 mL·min-1;柱温:25℃。结果:在所选定的色谱条件下,磺丁基-β-环糊精与β-环糊精能分离完全;β-环糊精在0.1～1.6 mg·mL-1内,峰面积与浓度线性关系良好,r=0.9999;最低检测限为2μg。结论:方法简便,准确,专属性强,可用于磺丁基-β-环糊精中的β-环糊精检测及含量测定质量控制。