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目的:建立同时测定抗菌消炎片中绿原酸、黄芩苷、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚含量的方法。方法:采用反向高效液相色谱法。色谱柱为Agilent Extend C18,流动相为乙腈-0.5%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长分别为327 nm(绿原酸)、280 nm(黄芩苷)和450 nm(芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚),柱温为30 ℃,进样量为10 μL。结果:绿原酸、黄芩苷、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚检测进样量线性范围分别为0.209 4~4.188 0 μg(r=0.999 9)、0.372 0~7.440 0 μg(r=0.999 9)、0.006 3~0.126 2 μg(r=0.999 9)、0.011 6~0.232 2 μg(r=0.999 9)、0.005 3~0.106 0 μg(r=0.999 8)、0.012 8~0.256 4 μg(r=0.999 9)、0.016 5~0.330 3 μg(r=0.999 8);定量限分别为2.01、1.93、0.76、1.25、1.24、0.53、1.53 ng,检测限分别为0.98、0.65、0.25、0.42、0.41、0.18、0.52 ng;加样回收率分别为98.41%~100.40%(RSD=0.76%, n=9)、96.17%~100.10%(RSD=1.58%,n=9)、96.11%~100.10%(RSD=1.33%,n=9)、96.29%~100.80%(RSD=1.85%,n=9)、96.88%~100.10%(RSD=1.22%,n=9)、97.81%~101.90%(RSD=1.64%,n=9)、96.46%~101.30%(RSD=1.85%,n=9)。结论:该方法准确可靠,重复性好,可用于抗菌消炎片中7种成分含量的同时测定。
OBJECTIVE: To develop a method for simultaneous determination of chlorogenic acid, baicalin, aloe emodin, rhein, emodin, chrysophanol and physcione in Kangjun xiaoyan tablets. METHODS: RP-HPLC method was adopted. The determination was performed on Agilent Extend C18 with mobile phase consisted of acetonitrile-0.5% phosohoric acid solution (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelengths were set at 327 nm (chlorogenic acid), 280 nm (baicalin) and 450 nm (aloe emodin, rhein, emodin, chrysophanol, physcione). The column temperature was 30 ℃, and sample size was 10 μL. RESULTS: The linear ranges of chlorogenic acid, baicalin, aloe emodin, rhein, emodin, chrysophanol and physcione were 0.209 4-4.188 0 μg(r=0.999 9),0.372 0-7.440 0 μg(r=0.999 9),0.006 3-0.126 2 μg(r=0.999 9),0.011 6-0.232 2 μg(r=0.999 9),0.005 3- 0.106 0 μg(r=0.999 8), 0.012 8-0.256 4 μg(r=0.999 9), 0.016 5-0.330 3 μg(r=0.999 8), respectively. The limits of quantitation were 2.01, 1.93, 0.76, 1.25, 1.24, 0.53 and 1.53 ng; the limits of detection were 0.98, 0.65, 0.25, 0.42, 0.41, 0.18 and 0.52 ng, respectively. The recoveries were 98.41%-100.40%(RSD=0.76%,n=9),96.17%-100.10%(RSD=1.58%,n=9),96.11%-100.10%(RSD=1.33%,n=9), 96.29%-100.80%(RSD=1.85%,n=9),96.88%-100.10%(RSD=1.22%,n=9),97.81%-101.90%(RSD=1.64%,n=9), 96.46%-101.30%(RSD=1.85%,n=9), respectively. CONCLUSIONS: The method is accurate, reliable and reproducible. It can be used for simultaneous determination of 7 components in Kangjun xiaoyan tablets.
抗菌消炎片反向高效液相色谱法绿原酸黄芩苷芦荟大黄素大黄酸大黄素大黄酚大黄素甲醚含量测定
Kangjun xiaoyan tabletsRP-HPLCChlorogenic acidBaicalinAloe emodinRheinEmodinChrysophanolPhyscioneContent detcrmination
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