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建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定首乌藤中二苯乙烯(二苯乙烯苷、虎杖苷、白藜芦醇)、蒽醌(大黄素、大黄素甲醚、大黄素-8-β-D-葡萄糖苷、芦荟大黄素)、黄酮(表儿茶素、芦丁、金丝桃苷、紫云英苷、槲皮素)及酚酸(没食子酸)等13种成分的方法。采用Waters BEH C18(2.1 mm×100 mm,1.7μm)色谱柱,流动相为水(含0.1%甲酸)-乙腈,梯度洗脱,柱温35℃,流速0.25 m L·min~(-1),采用电喷雾离子源(ESI),多反应离子监测(MRM)扫描方式进行检测。采用TOPSIS法对13种成分进行分析评价。结果 13种成分在一定浓度范围内均呈良好的线性关系,相关系数大于0.991 5,精密度、重复性和稳定性良好;加样回收率在95.24%~102.3%,RSD均小于5%。TOPSIS分析显示广州产的样品综合质量较好。所建立的方法准确、专属性、重复性较好,可用于首乌藤中多元功效物质或指标成分的同时测定,为首乌藤药材内在质量的综合评价和全面控制提供新的方法参考。
To establish a simultaneous determination method for stilbene (stilbene glycoside, polydatin, resveratrol), anthraquinone (emodin, emodin A) by UPLC-MS / MS Ether, emodin -8-β-D-glucoside, aloe-emodin), flavonoids (epicatechin, rutin, hyperoside, 13 kinds of ingredients such as methods. The mobile phase was water (containing 0.1% formic acid) -acetonitrile with a gradient of BEH C18 (2.1 mm × 100 mm, 1.7 μm) and the column temperature was 35 ℃ and the flow rate was 0.25 m L · min -1 , Using electrospray ionization source (ESI), multi-reactive ion monitoring (MRM) scan detection. The TOPSIS method was used to analyze and evaluate 13 components. Results The 13 components all showed a good linearity within a certain concentration range. The correlation coefficient was greater than 0.991 5. The precision, repeatability and stability were good. The average recoveries were 95.24% -102.3% with RSD less than 5%. TOPSIS analysis shows that the quality of the samples produced in Guangzhou is better. The established method is accurate, specific and reproducible. It can be used for the simultaneous determination of multivariate metabolites or index components in Polygonum pentaphyllum for the first time, providing a new method reference for the comprehensive evaluation and comprehensive control of the intrinsic quality of Polygonum morifolium.