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目的:建立小叶黄杨中紫丁香苷和香草酸的TLC鉴别和HPLC含量测定方法,研究药材中不同部位紫丁香苷和香草酸的含量差异。方法:TLC鉴别法,使用硅胶GF254薄层板,以三氯甲烷-甲醇-甲酸(8∶1.2∶0.5)作为展开剂;HPLC法,使用Xbridge C_(18)色谱柱(4.6 mm×250 mm,5μm),以甲醇-0.2%磷酸水溶液(17∶83)为流动相,流速1 m L·min~(-1),检测波长264 nm,柱温35℃。结果:TLC法操作简便,准确,斑点清晰,专属性好。紫丁香苷、香草酸质量浓度分别在3.36~302.4和0.55~695.5μg·m L~(-1)(r=0.999 5)范围内线性关系良好,3种浓度水品平均回收率分别在99.8%~103.0%和98.4%~101.1%范围内。小叶黄杨不同部位中紫丁香苷和香草酸的含量存在差异,紫丁香苷在粗茎、细枝、叶和地上部分中的含量分别为0.030~0.324、0.002~0.518、0.013~0.907和0.010~0.667 mg·g~(-1),香草酸在粗茎、细枝、叶和地上部分中的含量分别为0.025~0.077、0.021~0.087、0.012~0.132和0.020~0.123 mg·g~(-1)。结论:该方法能鉴别小叶黄杨,准确测定紫丁香苷和香草酸的含量,为开发利用小叶黄杨资源提供了科学依据。
OBJECTIVE: To establish TLC identification and HPLC determination of syringin and vanillic acid in Euonymus japonicus, and to study the content differences of syringin and vanillic acid in different parts of medicinal materials. METHODS: TLC analysis was performed on a silica gel GF254 TLC plate with chloroform-methanol-formic acid (8: 1.2: 0.5) as developing solvent. HPLC was performed on a Xbridge C 18 column (4.6 mm × 250 mm, The mobile phase was methanol-0.2% phosphoric acid solution (17:83) with a flow rate of 1 mL · min -1. The detection wavelength was set at 264 nm and the column temperature was 35 ℃. Results: TLC method is simple, accurate, clear spots, good specificity. The calibration curves of syringin and vanillic acid showed good linearity in the range of 3.36 ~ 302.4 and 0.55 ~ 695.5μg · m L -1 (r = 0.999 5) respectively. The average recoveries of syringol and vanillic acid were 99.8% ~ 103.0% and 98.4% ~ 101.1%. The content of syringin and vanillic acid in different parts of Euonymus japonicas was different. The content of syringin in stem, twig, leaf and aerial parts were 0.030-0.332, 0.002-0.518, 0.013-0.907 and 0.010-0.667 mg, respectively · G ~ (-1). The contents of vanillic acid in the stems, twigs, leaves and aerial parts were 0.025 ~ 0.077, 0.021 ~ 0.087, 0.012 ~ 0.132 and 0.020 ~ 0.123 mg · g ~ (-1), respectively. Conclusion: This method can identify Euonymus japonicus, accurately determine the content of syringin and vanillic acid, and provide a scientific basis for the development and utilization of Euonymus japonicus.