中药山蜡梅叶质量标准研究

Study on Quality Standard of Chimonanthus nitens Leaf

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、口．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（250mm×4．6mm，5μm）色谱柱，流动相为乙腈．水，梯度洗脱，流速1．0mL／min，检测波长344nm，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 set up the quality standard of Chimonanthus nitens leaf. Methods： Five compounds were identified by double-development thin layer chromatography ,the plate was colorized with 1% vanillin-H2SO4 solution and warmed up in 110℃ ; The content of four compounds was determined by HPLC, the chromatography separation was performed on the Elite hypersil ODS2 （ 250 mm × 4. 6 mm ,5 μm）column with gradient elution. The mixture of acetonitrile and water as the mobile phase at a flow rate of 1.0 mL/min was used,the detection wavelength was 344 nm and the column temperature was set at 40℃. Results： The TLC identification was highly specific and spots were clear. In HPLC method, the calibration curve was linear in the range of 5. 665 - 56. 65 μg/mL for scopoletin （ r =0. 9999） ,the average recovery, was 97.06% and RSD was 1.27% ; The calibration curve was linear in the range of 2. 4312 - 24. 312 μg/mL for isofraxidin （r =0. 9999） ,the average recovery was 102. 86% and RSD% was 0. 93% ; The calibration curve presented a linear range from 2. 444 - 24.44 μg/ mL for scoparone （r =0. 9999） ,the average recovery was 102. 18% and RSD was 1.81%. The standard curve presented a linear range from 9. 012 - 90. 12 μg/mL for rutin （r =0. 9992） ,the average recovery was 104. 44% and RSD was 4. 2%. Conclusion： These methods are reproducible, sensitive and simple and can be used to control the quality of Chimonanthus nitens leaf.