1. 温州医科大学药学院,浙江,温州,325005
2. 浙江省亚热带作物研究所,浙江,温州,325005
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包晓青, 吴志刚, 严鹏程, 等. 铁皮石斛中芪类成分的分离及含量测定[J]. 上海中医药杂志, 2015,49(2):86-89.
BAO Xiao-qing, WU Zhi-gang, YAN Peng-cheng, et al. Separation and determination of stilbenes ingredients in Dendrobii Officialis Caulis[J]. Shanghai Journal of Traditional Chinese Medicine, 2015,49(2):86-89.
目的:分离制备铁皮石斛质量指标性成分,并建立其含量的高效液相测定方法 方法:硅胶、Sephadex LH-20等色谱学方法分离纯化铁皮石斛,波谱学特征鉴定化合物的结构;高效液相色谱法测定3,4-二羟基-5,4’-二甲氧基联苄 (DDB-1) 的含量, Phenomenex C,18,色谱柱 (250 mm×4.60 mm,5 μm),以乙腈-水溶液为流动相进行梯度洗脱,检测波长为230 nm 结果:共分离得到四个芪类化合物,分别为:3,4-二羟基-5,4’-二甲氧基联苄;3,4’-二羟基-5-甲氧基联苄;5-羟基-3,4’-二甲氧基联苄;4’-羟基-3’,5’-二甲氧基联苄。从中选取3,4-二羟基-5,4’-二甲氧基联苄 (DDB-1) 作为指标性成分,其在0.044~0.44 μg范围内呈现良好的线性关系(R,2, = 0.999 9);不同种植基地的DDB-1含量差异较大,不同采收月份(3月份到5月份)的铁皮石斛中DDB-1含量差异不太明显 结论:本研究建立的含量测定方法准确、可靠、简便,可用于铁皮石斛中DDB-1含量测定,为铁皮石斛质量评价提供了参考依据。
Objective:To separate chemical indicator and establish a HPLC method for determining the indicator in herbs from Dendrobii Officialis Caulis Methods:The constituents were separated and purified by column chromatography on silica gel and Sephadex LH-20, as well as the chemical structures were determined by spectral data analyses. Determination of content of 3,4-dihydroxy-5,4’-dimethoxy bibenzyl (DDB-1) was performed by using high performance liquid chromatography. A Phenomenex-C,18, column (250 mm × 4.60 mm, 5 μm) was adopted with a mobile phase of acetonitrile-water, the runs were set at 230 nm Results:Four stilbenoids compounds were isolated and identified as 3,4-dihydroxy-5,4’-dimethoxybibenzyl, 3,4-dihydroxy-5-methoxybibenzyl, 5-hydroxy-3,4’-dimethoxybibenzyl, 4’-hydroxy-3’, 5’- dimethoxybibenzyl. DDB-1 was selected as an indicator to assess the quality of Dendrobii Officialis Caulis. This indicator showed a good linear relationship within the range of 0.044 ~ 0.44 μg (R,2,=0.999 9). The determination of DDB-1 in tested samples from different production base was most different, and it had little difference between each other if Dendrobii Officialis Caulis harvested in different month Conclusion:This proposed method was found to be accurate, reliable and simple, providing rapid and special determination of DDB-1, which could be used to control quality of Dendrobii Officialis Caulis.
铁皮石斛含量测定34-二羟基-54’-二甲氧基联苄高效液相色谱法
Dendrobii Officialis Caulisdetermination34-dihydroxy-54’-dimethoxy bibenzylHPLC
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