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目的:建立同时测定冬凌草片中冬凌草甲素、冬凌草乙素和迷迭香酸含量的方法。方法:采用高效液相色谱切换波长法,以冬凌草甲素为基准峰,分别计算冬凌草乙素和迷迭香酸与冬凌草甲素的相对校正因子,用校正因子计算冬凌草乙素和迷迭香酸的含量。色谱柱为Phenomenex C18,流动相为乙腈-0.2%磷酸(梯度洗脱),流速为1.0 ml/min,检测波长为239(0~20 min,冬凌草乙素)、329(20~25 min,迷迭香酸)、239 nm(25~49 min,冬凌草甲素),柱温为40 ℃,进样量为10 μl。结果:冬凌草甲素、冬凌草乙素和迷迭香酸检测进样量线性范围分别为41.6~623.4(r=0.999 9)、13.8~207.2(r=0.999 9)、36.8~552.0 ng(r=0.999 9);精密度、稳定性、重复性试验的RSD<3%;加样回收率分别为99.6%~102.5%(RSD=1.1%,n=6)、98.8%~101.4%(RSD=1.0%,n=6)、99.0%~102.5%(RSD=1.5%,n=6)。结论:该方法操作简便、稳定、重复性好,可用于同时测定冬凌草片中冬凌草甲素、冬凌草乙素和迷迭香酸的含量。
OBJECTIVE:To establish a method for simultaneous determination of oridonin, ponicidin and rosemary acid in Donglingcao tablet. METHODS: With the reference peak of oridonin, HPLC with changingwavelength method was conducted to calculate the relative correction factors of ponicidin and rosemary acid, which were used to calculate the contents of ponicidin and rosemary acid. The column was Phenomenex C18 with mobile phase of acetonitrile - 0.2% phosphoric acid (gradient elution) at a flow rate of 1.0 ml/min, detection wavelength was 239 nm(0-20 min,ponicidin),329 nm(20-25 min,rosemary acid),239 nm(25-49 min,oridonin),the column temperature was 40 ℃,and the injection volume was 10 μl. RESULTS: The linear range was 41.6-623.4 ng(r=0.999 9) for oridonin,13.8-207.2 ng(r=0.999 9) for ponicidin, 36.8-552.0 ng(r=0.999 9) for rosemary acid. RSDs of precision, stability and reproducibility tests were lower than 3%, recovery was 99.6%-102.5%(RSD=1.1%,n=6)、98.8%-101.4%(RSD=1.0%,n=6)、99.0%-102.5%(RSD=1.5%,n=6). CONCLUSIONS: The method is simple, stable and reproducible, and can be used for the simultaneous determination of oridonin, ponicidin and rosemary acid in Donglingcao tablet.
冬凌草片切换波长一测多评冬凌草甲素冬凌草乙素迷迭香酸
Donglingcao tabletsChangingwavelengthMulti-components quantitative analysisby one markerOridoninPonicidinRosemary acid
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