摘要
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 the methods of TLC identification and HPLC determination of the contents of syringin and vanillic acid in Buxus sinica,and determine different contents of syringin and vanillic acid in different fractions of Buxus sinica.Methods：The thin-layer plate silica of gel GF254 and organic solvent chloroform-methanol-formic acid（8∶1.2∶0.5,v/v/v） were used in TLC identification.The HPLC method was performed on a Xbridge C18 chromatographic column（4.6 mm×250 mm,5 μm） with the mobile phase consisting of methanol-0.2% phosphoric acid solution（17∶83） at the flow rate of 1 m L·min^-1.The detection wavelength was set at 264 nm,and the column temperature was set at 35 ℃.Results：TLC method was simple and accurate,and the spots were clear with good separation.The linear range of syringin and vanillic acid were 3.36-302.4 and 0.55-695.5 μg·m L^-1（r=0.999 5）,and the recoveries on three concentration levels were 99.8%^（-1）03.0% and 98.4%^（-1）01.1% respectively.The contents of syringin and vanillic acid were obviously different in different parts of Buxus sinica.The contents of syringin in main stem,withe,leaves and aerial part were 0.030-0.324 mg·g^-1,0.002-0.518 mg·g^-1,0.013-0.907 mg·g^-1 and 0.010-0.667 mg·g^-1,respectively.The contents of vanillic acid in main stem,withe,leaves and aerial part were 0.025-0.077 mg·g^-1,0.021-0.087 mg·g^-1,0.012-0.132 mg·g^-1 and 0.020-0.123 mg·g^-1,respectively.Conclusion：The method can be used to identify Buxus sinica effectively,and to determine the contents of syringin and vanillic acid in different parts accurately,which provides a scientific basis for development and utilization Buxus sinica resources.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2017年第2期304-309,共6页
Chinese Journal of Pharmaceutical Analysis
基金
贵州省科学技术基金(黔科合J字[2013]2032号)
作者简介
Tel：15285167124；E—mail：1274191418@qq．com
通信作者Tel：13368610577；E-mail：1074459931@qq．com
