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目的:建立山蜡梅叶的质量标准。方法:采用二次展开薄层色谱法同时鉴别桉油精、β-石竹烯、芳樟醇、东莨菪内酯、滨蒿内酯,显色剂为1%香草醛硫酸溶液,烘烤温度为110℃;采用HPLC法同时测定东莨菪内酯、异嗪皮啶、滨蒿内酯、芦丁的含量,使用依利特Hypersil ODS2(250 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-水,梯度洗脱,流速1.0 mL/min,检测波长344 nm,柱温为40℃。结果:TLC色谱中5个化合物的斑点清晰,特征明显。HPLC法中东莨菪内酯在5.665~56.65μg/mL浓度范围内线性关系良好,r=0.9999,平均回收率为97.06%,RSD为1.27%(n=6);异嗪皮啶在2.4312~24.312μg/mL范围线性关系良好,r=0.9999,平均回收率为102.86%,RSD为0.93%(n=6);滨蒿内酯在2.444~24.44μg/mL范围线性良好,r=0.9999,平均回收率为102.18%,RSD为1.81%(n=6);芦丁在9.012~90.12μg/mL范围线性良好,r=0.9992,平均回收率为104.44%,RSD为4.2%(n=6)。结论:该方法操作简便,结果准确,重复性好,可用来控制山蜡梅叶的质量。
Objective: To establish the quality standard of Methods: The elution method of eucalyptol, β-caryophyllene, linalool, scopoletin and scopolactone was established by the secondarily developed thin-layer chromatography. The curing agent was 1% vanillin-sulfuric acid solution. The baking temperature was 110 ℃. The contents of scopoletin, isoxapide, scoparone and rutin were determined simultaneously by HPLC. The elution was carried out on a Hypersil ODS2 column (250 mm × 4.6 mm, 5 μm) with a mobile phase of acetonitrile- Water, gradient elution, flow rate 1.0 mL / min, detection wavelength 344 nm, column temperature 40 ℃. Results: The five compounds in TLC showed clear spots and obvious features. The linear range of scopolactone was 5.665 ~ 56.65μg / mL. The average recovery was 97.06% with a RSD of 1.27% (n = 6). The isoindopidine concentration ranged from 2.4312 to 24.312μg (r = 0.9999), the average recovery was 102.86%, and the RSD was 0.93% (n = 6). The linear range was 2.444 ~ 24.44μg / mL, and the average recovery was (N = 6). The average RSD of rutin was 104.44% and the RSD was 4.2% (n = 6). The average recovery of rutin in the range of 9.012 ~ 90.12 μg / mL was r = 0.9992. Conclusion: The method is simple, accurate, reproducible and can be used to control the quality of the leaves.