便通胶囊的含量测定及化学模式识别分析
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篇名: 便通胶囊的含量测定及化学模式识别分析
TITLE: Content determination and chemical pattern recognition analysis of Biantong capsules
摘要: 目的 建立同时测定便通胶囊中芸香柚皮苷等11个成分含量的方法,进行化学模式识别分析,筛选差异标志物。方法采用高效液相色谱法。以VenusilXBPC18为色谱柱,乙腈-0.1%磷酸溶液为流动相进行梯度洗脱,流速为1.0mL/min,进样量为10µL,柱温为30℃,检测波长分别为283、330、520、220nm。以毛蕊花糖苷为内参物,结合一测多评法测定含量,并与外标法结果进行比较。采用SPSS26.0、SIMCA14.1软件进行聚类分析、主成分分析和正交偏最小二乘法-判别分析,以变量重要性投影(VIP)值大于1为标准筛选影响便通胶囊质量的差异标志物。结果高效液相色谱结合一测多评法测得芸香柚皮苷、柚皮苷、新橙皮苷、松果菊苷、管花苷A、异毛蕊花糖苷、矢车菊素-3-O-葡萄糖苷、矢车菊素-3-O-芸香糖苷、白术内酯Ⅲ、白术内酯Ⅰ的含量分别为0.739~1.265、1.134~2.158、1.407~2.359、1.368~2.502、0.304~0.522、0.257~0.521、0.423~0.727、0.375~0.733、0.130~0.283、0.062~0.166mg/g,与外标法测定结果的相对平均偏差均小于2%。聚类分析结果显示,15批样品可聚为3类,S1~S7为一类,S8~S10为一类,S11~S15为一类,与主成分分析的分类结果一致。正交偏最小二乘法-判别分析结果显示,矢车菊素-3-O-芸香糖苷、白术内酯Ⅲ、柚皮苷、新橙皮苷、松果菊苷、毛蕊花糖苷的VIP值大于1。结论成功建立了同时测定便通胶囊中芸香柚皮苷等11个成分含量的方法,结合化学模式识别分析可用于便通胶囊的质量控制。矢车菊素-3-O-芸香糖苷等6个成分可能是影响便通胶囊质量的差异标志物。
ABSTRACT: OBJECTIVE To establish the method for simultaneous determination of 11 components as narirutin in Biantong capsules,to conduct chemical pattern recognition analysis and to screen differential markers affecting their quality . METHODS HPLC method was adopted . The separation was carried out on Venusil XBP C 18 column with mobile phase consisted of acetonitrile - 0.1% phosphoric acid solution with gradient elution at flow rate of 1.0 mL/min. The sample size was 10 µL,and column temperature was set at 30 ℃. The detection wavelengths were set at 283,330,520,220 nm,respectively. Using verbascoside as an internal standard ,the contents were determined by quantitative analysis of mult -components by single marker (QAMS),and the results were compared with those of external standard method . Cluster analysis ,principle component analysis and orthogonal partial least squares -discriminant analysis were performed with SPSS 26.0 and SIMCA 14.1 software. The differential markers affecting the quality of Biantong capsules were screened using the variable importance in projection (VIP)value greater than 1 as the standard . RESULTS The contents of narirutin ,naringin,neohesperidin,echinacoside,tubuloside A ,isoacteoside,cyanidin-3-O-glucoside, cyanidin-3-O-rutoside,atractylolide Ⅲand atractylolide Ⅰ were 0.739-1.265,1.134-2.158,1.407-2.359,1.368-2.502,0.304-0.522, 0.257-0.521,0.423-0.727,0.375-0.733,0.130-0.283 and 0.062-0.166 mg/g,respectively. The relative average deviation of them from the external standard method was less than 2%. The results of cluster analysis showed that 15 batches of samples could be grouped into three categories ,S1-S7 as a category ,S8-S10 as a category ,and S 11-S15 as a category ,which was consistent with the classification results of principal component analysis . The results of orthogonal partial least squares -discriminant analysis showed that the VIP values of cyanidin -3-O-rutoside,atractylolide Ⅲ, naringin,neohesperidin,echinacoside and verbascoside were all greater than 1. CONCLUSIONS The method for simultaneous determination of 11 components in Biantongcapsules, including narirutin , is successfully established . Combined with chemical pattern recognition analysis ,it can be used for the quality control of Biantong capsules . Six components such as cyanidin -3-O-rutoside may be the differential markers that affect the quality of Biantong capsules .
期刊: 2022年第33卷第18期
作者: 舒波,雷果平,袁斌
AUTHORS: SHU Bo,LEI Guoping ,YUAN Bin
关键字: 便通胶囊;高效液相色谱法;一测多评法;化学模式识别;质量评价;差异标志物
KEYWORDS: Biantong capsules ;HPLC;QAMS;chemical pattern recognition ;quality evaluation ;differential markers
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