3-环己烯-1-甲酸的高效液相色谱手性分析

Chiral HPLC analytical method of cyclohex-3-ene-1-carboxylic acid

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.