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目的:采用2种纤维素衍生物手性固定相,比较并建立了肾上腺素、盐酸去氧肾上腺素对映体的拆分分析方法并探讨其机理。方法:色谱柱为CHIRALCEL OD-H和CHIRALCEL OJ-H(250 mm×4.6 mm,5μm);流动相:正己烷-异丙醇(含不同比例甲醇、三氟乙酸、二乙胺);检测波长:280 nm;流速:0.8mL.min-1;柱温:25℃。同时,考察了有机添加剂酸和碱的比例、醇置换剂的类型和比例及温度对上述化合物分离的影响,同时对分离机理进行了阐述。结果:肾上腺素在纤维素衍生物手性固定相正相条件下分离度为1.56,盐酸去氧肾上腺素分离度为2.30。对映体的色谱保留和分离度通过改变流动相中醇类置换剂的浓度、有机改性剂酸和碱的浓度、柱温、流速等因素调节。分离度随醇置换剂浓度减小或流速的降低而增加,有机改性剂酸和碱的浓度分别为0.1%、0.05%,分离度峰形好,样品在柱温25℃时分离度最好,并保持温度不变,以得到稳定的分离结果。结论:肾上腺素、盐酸去氧肾上腺素两种药物在纤维素衍生物手性固定相上能得到良好分离。此种分析方法准确快速、灵敏,操作简单。
OBJECTIVE: To compare and establish the separation and analysis methods of epinephrine and phenylephrine hydrochloride enantiomers by using two kinds of cellulose derivatives as chiral stationary phases, and to explore their mechanism. METHODS: The chromatographic columns were CHIRALCEL OD-H and CHIRALCEL OJ-H (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of n-hexane and isopropanol with different ratios of methanol, trifluoroacetic acid and diethylamine. : 280 nm; flow rate: 0.8 mL.min-1; column temperature: 25 ° C. At the same time, the effects of the ratio of organic acid and alkali, the type and proportion of alcohol displacer, and the temperature on the separation of the above compounds were investigated. At the same time, the separation mechanism was discussed. Results: The resolution of epinephrine was 1.56 in the normal phase of the cellulose derivative chiral stationary phase and 2.30 in the phenylephrine hydrochloride. The chromatographic retention and resolution of the enantiomers were adjusted by varying the concentration of alcohol displacer in the mobile phase, the concentration of organic modifier acids and bases, column temperature, flow rate and the like. The degree of separation increased with the decrease of concentration of alcohol displacer or the decrease of flow rate. The concentrations of organic modifier acid and base were 0.1% and 0.05%, respectively. The peak of resolution was good. The best resolution was at 25 ℃ , And keep the temperature constant, in order to get a stable separation results. Conclusion: Both epinephrine and phenylephrine hydrochloride can be well separated on the chiral stationary phase of cellulose derivatives. This method of analysis is accurate, fast, sensitive and easy to use.