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作 者:许丽丽 王玉团 徐丽华 林永强 牛艳 XU Lili WANG Yutuan XU Lihua LIN Yongqiang NIU Yan(Shandong Institute for Food and Drug Control, Jinan 250101, China)
出 处:《中国药房》2017年第21期2981-2984,共4页China Pharmacy
基 金:山东省自然科学基金资助项目(No.ZR2013HM074)
摘 要: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 C_(18),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10μL。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 0μg(r=0.999 9)、0.372 0~7.440 0μg(r=0.999 9)、0.006 3~0.126 2μg(r=0.999 9)、0.011 6~0.232 2μg(r=0.999 9)、0.005 3~0.106 0μg(r=0.999 8)、0.012 8~0.256 4μg(r=0.999 9)、0.016 5~0.330 3μg(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.
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