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目的:建立HPLC波长切换法同时测定九味双解口服液中绿原酸、咖啡酸、木犀草苷、黄芩苷和大黄素的含量。方法:采用Shiseido Capcell Pak C_(18)(200 mm×4.6 mm,5μm)色谱柱,流动相为甲醇(A)-0.1%磷酸溶液(B)(梯度洗脱),流速为1.0 ml·min~(-1),柱温为25℃,检测波长(0~19 min,在327 nm波长下检测绿原酸;19~25 min,在323 nm波长下检测咖啡酸;25~35 min,在350 nm波长下检测木犀草苷;35~55 min,在320 nm波长下检测黄芩苷;55~60 min,在254 nm波长下检测大黄素)。结果:绿原酸、咖啡酸、木犀草苷、黄芩苷和大黄素的线性范围分别为0.34~6.81μg·ml~(-1)(r=0.999 9)、0.23~4.56μg·ml~(-1)(r=0.999 5)、1.32~26.38μg·ml~(-1)(r=0.999 9)、9.60~192.01μg·ml~(-1)(r=0.999 9)、1.14~22.80μg·ml~(-1)(r=0.999 6);平均加样回收率分别为99.50%(RSD=0.52%)、99.10%(RSD=1.43%)、98.83%(RSD=0.94%)、99.98%(RSD=0.21%)、99.22%(RSD=0.82%)(n=9)。结论:本文建立的含量测定方法,具有操作简便、结果准确、重现性良好的特点,可用于九味双解口服液的质量控制。
OBJECTIVE: To establish a HPLC wavelength-switching method for simultaneous determination of chlorogenic acid, caffeic acid, luteolin, baicalin and emodin in Jiuwei Shuang-Xie oral solution. Methods: The mobile phase consisted of methanol (A) - 0.1% phosphoric acid solution (B) (gradient elution) on a Shiseido Capcell Pak C 18 (200 mm × 4.6 mm, 5 μm) column with a flow rate of 1.0 ml · min ~ (-1), column temperature was 25 ℃, detection wavelength (0 ~ 19 min, detection of chlorogenic acid at 327 nm wavelength; detection of caffeic acid at 323 nm wavelength for 19-25 min; detection of luteolin at nm wavelength; detection of baicalin at 320 nm at 35-55 min; detection of emodin at 254 nm at 55-60 min). Results: The linear ranges of chlorogenic acid, caffeic acid, luteolin, baicalin and emodin were 0.34 ~ 6.81μg · ml -1 (r = 0.999 9), 0.23 ~ 4.56μg · ml ~ (-1) (R = 0.999 5), 1.32 ~ 26.38μg · ml -1 (r = 0.999 9), 9.60 ~ 192.01μg · ml -1 (r = 0.999 9), 1.14 ~ 22.80μg · The average recoveries were 99.50% (RSD = 0.52%), 99.10% (RSD = 1.43%), 98.83% (RSD = 0.94%) and 99.98% (r = 0.999 6) RSD = 0.21%), 99.22% (RSD = 0.82%) (n = 9). Conclusion: The method for determination of content in this paper has the advantages of simple operation, accurate results and good reproducibility. It can be used for the quality control of Jiuwei Bisheng oral solution.