基于UPLC独一味中8种成分测定及其含量影响因素初步研究.docVIP

基于UPLC独一味中8种成分测定及其含量影响因素初步研究 　　[摘要] 建立同时测定独一味中胡麻属苷、山栀苷甲酯、绿原酸、咖啡酸、8-O-乙酰山栀苷甲酯、连翘酯苷B、木犀草苷和麦角甾苷8种成分含量的方法。采用Kinetex XB-C18色谱柱（4.6 mm×50 mm，2.6 μm）以乙腈（A）-0.1%磷酸溶液（B）为流动相进行梯度洗脱（0～10 min，6%～14.5% A；10～18.5 min，14.5%～17% A；18.5～23 min，17%～18% A），流速1.0 mL?min-1，检测波长238，320，350 nm，柱温30 ℃。结果发现8个成分分离度良好，在线性范围内呈现良好的线性关系（r≥0.999 8），平均加样回收率96.61%～100.4%。该方法操作简便，专属性好，精密度高，可用于独一味药材的鉴别及质量评价。研究表明，独一味各类成分之间具有相关性；产地是影响独一味成分含量的主要因素；退化梯度对其含量影响不明显；样品储藏一年后胡麻属苷含量显著降低。 　　[关键词] 独一味； 超高效液相色谱； 含量测定； 环烯醚萜苷； 苯乙醇苷 　　[Abstract] To establish a method for simultaneous determination of the contents of sesamoside， menthyl chloride， chlorogenic acid， caffeic acid， 8-O-acetyl-phloridzin methyl ester， forsythiaside B， luteolin， and ergosterol， the LIPLC analysis was performed on a Kinetex XB-C18 （4.6 mm×50 mm，2.6 μm）column with acetonitrile （A）-0.1% phosphoric acid solution （B） as the mobile phase. The flow rate is 1.0 mL min-1. The detection wavelength was 238， 320 and 350 nm and column temperature was 30 ℃. The results showed that the eight components could be completely separated with good linear relationships （r ≥ 0.999 8） in the linear range. The average recoveries were 96.61% -100.4%. The method was simple with strong specificity and high precision. It can be used for the identification and quality evaluation of the Lamiophlomis rotate.The results also showed that there was a correlation between the various components， and the habitat was the main factor affecting the content of the eight components. However， the degradation gradient had no obvious effect on the contents， while the content of sesamoside was significantly decreased after one year of storage. 　　[Key words] Lamiophlomis rotate； UPLC； contents determination； iridoid glycosides； phenethyl alcohol glycoside 　　??一味Lamiophlomis rotata （Benth.）Kudo为唇形科独一味属植物，藏语称“大巴”、“打布巴”，主要分布于我国中西部地区如西藏、青海、甘肃和四川等地，海拔2 700～4 500 m的高原或高山上强度风化的碎石滩中或石质高山草甸、河滩地。独一味为藏族、蒙古族、纳西族等少数民族常用草药，具有活血止血，祛风止痛之功效，用于跌打损伤，外伤出血，风湿痹痛，黄水病等[1]。近年来独一味显著的镇痛作用备受关注[2-3]，现有胶囊和分散片等多