摘要
目的研究3-环己烯-1-甲酸的高效液相色谱(HPLC)手性分析方法。方法正相条件下筛选3款常用的多糖衍生物型手性固定相并对分离结果进行优化。结果采用具有良好选择性的纤维素-三(4-甲基苯甲酸酯)涂覆型手性柱(250 mm×4.6 mm,5μm),在流动相为正己烷-异丙醇-三氟乙酸(体积比98∶2∶0.1),流速为0.5 mL·min-1,检测波长为200nm的条件下可以基线分离3-环己烯-1-甲酸消旋体,并能准确地检测对映体的纯度。结论相比以往样品需衍生后再用HPLC分析的方法,该方法更加简单、高效。
Objective To develop chiral HPLC analytical method of cyclohex-3-ene-1-carboxylic acid. Method Under normal-phase, three most useful chiral stationary phases based on polysaccharide derivatives were screened, and the resolution result was optimized. Result Chiral column(250 mm×4.6 mm, 5 μm) coated with cellulose tris(4-methylbenzoate) exhibited a good selectivity. The cyclohex-3-ene-1-carboxylic acid racemate could be separated from the baseline with the mobile phase of hexane-isopropanol-trifluoroacetic acid(V∶V∶V =98∶2∶0.1), flow rate of 0.5 mL?min-1 and the detection wavelength at 200 nm. The enantiomeric purities of(R)-and(S)-products were detected well. Conclusion This method is easier and more efficient compared with previous chiral HPLC analytical method which needs additional derivation.
作者
方钦虎
FANG Qinhu(Zhejiang Starry Pharmaceutical Co.,Ltd.,Taizhou 317300,China)
出处
《中国药剂学杂志(网络版)》
2019年第2期28-32,共5页
Chinese Journal of Pharmaceutics:Online Edition