In this study, a new enantioseparation method was established for the quantitative analysis of the oxypeucedanin enantiomers by using cellulose tris(3,5-dichlorophenyl carbamate) stationary phase column Chiralpak IC. For this method, enantiomeric separation of oxypeucedanin was achieved with the mobile phase consisting of acetonitrile-water (60:40, v/v) at a flow rate of 0.5 mL/min by changing the type and proportion of mobile phase. And the quantitative determination of racemic oxypeucedanin in Angelica Dahuricae Radix (in vitro) and rat plasma (in vivo) were performed on above-mentioned condition by High Performance Liquid Chromatography combined with diode arrangement detector (HPLC-DAD) and mass spectrometry (HPLC-MS/MS). The precision, repeatability, stability, recovery were within the acceptance criteria. And the method was validated in the concentration range of 1-400 μg/mL for the two enantiomers in vitro and 0.2–600 ng/mL in vivo. After validation, the established method was successfully applied to the stereoselective analysis of racemic oxypeucedanin in Angelica dahurica from different regions and the stereoselective pharmacokinetic investigation in rat. Results showed that the (+)-oxypeucedanin was at a relative high level in Angelica dahuricae Radix and (−)-oxypeucedanin performed a higher plasma concentration, which demonstrated the difference of oxypeucedanin enantiomers both in vitro and in vivo.

本研究采用纤维素三(3,5-二氯苯基氨基甲酸酯)固定相柱Chiralpak IC，建立了一种新的对映体分离方法，用于定量分析山毛榉素对映体。对于该方法，通过改变流动相的类型和比例，以 0.5 mL/min 的流速使用由乙腈-水 (60:40, v/v) 组成的流动相，实现了 oxypeucedanin 的对映体分离。并在上述条件下采用高效能法定量测定白芷（体外）和大鼠血浆（体内）中的外消旋长胡桃素。 液相色谱结合二极管排列检测器 (HPLC-DAD) 和质谱 (HPLC-MS/MS)。精密度、重复性、稳定性、回收率均在可接受标准范围内。该方法在两种对映体的体外浓度范围为 1-400 μg/mL 和体内浓度范围为 0.2-600 ng/mL 进行了验证。经验证，所建立的方法成功地应用于不同产地白芷中外消旋山茱萸素的立体选择性分析和大鼠立体选择性药代动力学研究。结果表明，白芷中的(+)-oxypeucedanin含量较高，(-)-oxypeucedanin的血浆浓度较高，证明了oxypeucedanin对映体在体外和体内的差异。