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机构地区:[1]中国科学院上海有机化学研究所
出 处:《分析化学》2007年第7期1043-1046,共4页Chinese Journal of Analytical Chemistry
摘 要:采用高效液相色谱法在大环糖肽抗生素键合固定相手性柱上拆分了卡巴拉汀(Rivastigmine)对映体。考察了甲醇:乙酸:三乙胺流动相体系中乙酸和三乙胺的浓度和比例、有机酸的种类、分离温度及流动相流速对拆分结果的影响。选定的色谱条件为:Chirobiotic V手性柱(250mm×4.6mmi.d.,5μm),流动相为y(甲醇):y(乙酸):V(三乙胺)=100:0.02:0.01,柱温5℃,流速0.5mL/min,检测波长274nm。在柱温5~30℃范围内测定lnα与1/T呈线性关系:lnα=△△H^0/RT+△△R^0/R。Direct enantioseparation of rivastigmine was achieved by high performance liquid chromatography using a vancomycin bound chiral stationary phase. The effects of the content and ratio of acetic acid/triethylamine in the mobile phase, acid additive, column temperature and flow rate of mobile phase on the enantioseparation of rivastigmine were studied. By using the Chirobiotic V column (250 mm × 4.6 mm i. d. , 5 μm), and methanol:acetic acid: triethylamine (100:0.02:0.01, V/V) as mobile phase, flow rate of 0.5 mL/min, detection wavelength of 274 nm, enantioseparation of rivastigmine was achieved. The relation- ship between lnα and 1/T was investigated in the range of 5 -30℃. The linear equation is lnα = ΔΔH^0/RT + ΔΔS^0 / R.
关 键 词:高效液相色谱法 对映体拆分 手性固定相 卡巴拉汀
分 类 号:R917[医药卫生—药物分析学]
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