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目的:建立同时测定益肾衍嗣丸中阿魏酸、梓醇、大黄素和大黄素甲醚含量的方法。方法:采用双波长高效液相色谱法。色谱柱为Kromasil-C18,流动相为甲醇-0.1%磷酸溶液(78 ∶ 22,V/V),流速为1.0 mL/min,检测波长为 280 nm(阿魏酸、大黄素和大黄素甲醚)、210 nm(梓醇),柱温为30 ℃,进样量为10 μL。结果:阿魏酸、梓醇、大黄素和大黄素甲醚检测质量浓度线性范围分别为0.090 8~2.270 0 μg/mL(r=0.999 9)、0.199 0~4.975 0 μg/mL(r=0.999 3)、0.354 0~8.850 0 μg/mL(r=0.999 9)、0.336 0~8.400 0 μg/mL(r=0.999 7);定量限分别为14.66、8.75、10.26、13.68 ng,检测限分别为5.66、2.67、3.78、4.25 ng;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为101.15%~102.73%(RSD=0.58%,n=6)、99.20%~101.69%(RSD=1.20%,n=6)、100.90%~101.36%(RSD=0.16%,n=6)、95.64%~98.96%(RSD=1.49%,n=6)。结论: 该方法准确可靠,操作简单,适用于益肾衍嗣丸中4种成分含量的同时测定。
OBJECTIVE: To establish a method for simultaneous determination of ferulic acid, catalpol, emodin and emodin methylether in Yishen yansi pills. METHODS: Double wavelength HPLC method was adopted. The separation was performed on Kromasil-C18 column with mobile phase methanol-0.1% phosphate solution (78 ∶ 22,V/V) at flow rate of 1.0 mL/min. The detection wavelengths were set at 210 nm for catalpol, 280 nm for ferulic acid, emodin and emodin methylether. The column temperature was 30 ℃, and sample size was 10 μL. RESULTS: The linear ranges were 0.090 8-2.270 0 μg/mL for ferulic acid (r=0.999 9), 0.199 0-4.975 0 μg/mL for catalpol (r=0.999 3), 0.354 0-8.850 0 μg/mL for emodin (r=0.999 9), 0.336 0~8.400 0 μg/mL for emodin methylether (r=0.999 7), respectively. The limits of quantitation were 14.66, 8.75, 10.26, 13.68 ng, and the limits of detection were 5.66, 2.67, 3.78, 4.25 ng, respectively. RSDs of precision, stability and reproducibility tests were lower than 2.0%. The recoveries were 101.15% -102.73%(RSD=0.58%,n=6), 99.20%-101.69%(RSD=1.20%,n=6),100.90%-101.36%(RSD=0.16%,n=6),95.64%-98.96%(RSD=1.49%,n=6), respectively. CONCLUSIONS: The method is accurate, reliable, simple and suitable for simultaneous determination of 4 kinds of components in Yishen yansi pills.
高效液相色谱法双波长益肾衍嗣丸阿魏酸梓醇大黄素大黄素甲醚含量
HPLCDouble wavelengthYishen yansi pillsFerulic acidCatalpolEmodinEmodin methyletherContent
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