Tian Shuge, Shi Yang, Yu Qian, Upur Halmurat
Xinjiang Key Laboratory of Famous Prescription and Science of Formulas, Urumqi-830011, Xinjiang, College of TCM, Xinjiang Medical University, Urumqi-830011, Xinjiang, China.
Pharmacogn Mag. 2010 Apr;6(22):116-9. doi: 10.4103/0973-1296.62898. Epub 2010 May 5.
A simple, precise, rapid and accurate, binary-phase high performance liquid chromatographic method has been developed for the determination of oleanolic acid and ursolic acid contents in the Ziziphora clinopodioides Lam. with short run time. Chromatographic separation is achieved by using HPLC system consisting of a Shimadzu LC-6AD and Kromasil C(18) column (150 x 4.6 mm, 10 mum, with pre-column), the mobile phase consists of methanol and 0.03 M phosphate buffer (pH = 3, 90:10). Detection wavelength is 214 nm. The speed of flow is 0.5 ml/min. The specimen handing quantity is 10 mul. The oleanolic acid's linearity range is 0.4 ~ 1.2 mg/ml (r = 0.9996). The ursolic acid's linearity range is 0.6 ~ 1.8 mg/ml (r = 0.9996), and the linear relationship is accurate. The average recovery (n = 6) of oleanolic acid is 99.5% (RSD = 1.19%) and ursolic acid is 102.3% (RSD = 1.25%). The content of oleanolic acid and ursolic acid in Ziziphora clinopodioides are 0.76 mg/g and 1.176 mg/g, respectively. The developed HPLC method can therefore be applied to both in vitro studies of oleanolic acid and ursolic acid formulations as well as drug estimation in biological samples.
已开发出一种简单、精确、快速且准确的二元相高效液相色谱法,用于测定短柄薄荷中齐墩果酸和熊果酸的含量,且运行时间短。采用由岛津LC - 6AD和Kromasil C(18)柱(150×4.6 mm,10μm,带预柱)组成的高效液相色谱系统进行色谱分离,流动相由甲醇和0.03 M磷酸盐缓冲液(pH = 3,90:10)组成。检测波长为214 nm。流速为0.5 ml/min。进样量为10μl。齐墩果酸的线性范围为0.41.2 mg/ml(r = 0.9996)。熊果酸的线性范围为0.61.8 mg/ml(r = 0.9996),线性关系良好。齐墩果酸的平均回收率(n = 6)为99.5%(RSD = 1.19%),熊果酸为102.3%(RSD = 1.25%)。短柄薄荷中齐墩果酸和熊果酸的含量分别为0.76 mg/g和1.176 mg/g。因此,所开发的高效液相色谱法可应用于齐墩果酸和熊果酸制剂的体外研究以及生物样品中的药物测定。