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目的建立同时测定痛经丸中丹参素、川芎嗪、芍药苷、羟基红花黄色素A和阿魏酸5个化学成分含量的方法。方法采用高效液相色谱-二级管阵列检测器(HPLC-DAD)法,Waters Symmetry C18色谱柱(250mm×4.6 mm,5μm),以甲醇(A)和0.2%甲酸水溶液(B)为流动相进行梯度洗脱;流速为0.6 m L·min-1;柱温30℃;检测波长为280 nm(0~16 min),254 nm(16~19 min),403 nm(19~22 min),320 nm(22~30 min)。结果丹参素、川芎嗪、芍药苷、羟基红花黄色素A和阿魏酸分别在0.012~1.2μg、0.021~2.08μg、0.0212~2.12μg、0.0124~1.24μg、0.008~0.8μg质量浓度范围内与其峰面积呈良好的线性关系(r≥0.9997);平均加样回收率均大于98.0%;RSD为0.73%~1.40%。结论该方法快速、准确、重复性好,可用于痛经丸的质量控制。
Objective To establish a method for simultaneous determination of 5 chemical constituents of Danshensu, ligustrazine, paeoniflorin, hydroxysafflor yellow A and ferulic acid in the dysmenorrhea pill. Methods HPLC was performed on a Waters Symmetry C18 column (250 mm × 4.6 mm, 5 μm) using a mobile phase of high performance liquid chromatography-diode array detector (HPLC-DAD) with methanol (A) and 0.2% formic acid Gradient elution was performed at a flow rate of 0.6 m L · min-1 and a column temperature of 30 ℃. The detection wavelength was 280 nm (0-16 min), 254 nm (16-19 min), 403 nm (19-22 min) 320 nm (22 ~ 30 min). Results Danshensu, ligustrazine, paeoniflorin, hydroxysafflor yellow A and ferulic acid were in the range of 0.012 ~ 1.2μg, 0.021 ~ 2.08μg, 0.0212 ~ 2.12μg, 0.0124 ~ 1.24μg, 0.008 ~ 0.8μg And its peak area showed a good linear relationship (r ≥ 0.997); average recovery was greater than 98.0%; RSD 0.73% ~ 1.40%. Conclusion The method is rapid, accurate and reproducible. It can be used for quality control of dysmenorrhea pill.