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便通胶囊的含量测定及化学模式识别分析 Δ
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舒 波 ,雷果平 ,袁 斌 (1.川北医学院附属医院药剂科,四川 南充 637000;2.南充市食品药品检验所,四
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川 南充 637000;3.川北医学院药物研究所,四川 南充 637000)
中图分类号 R917 文献标志码 A 文章编号 1001-0408(2022)18-2209-06
DOI 10.6039/j.issn.1001-0408.2022.18.07
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Venusil XBP C18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1.0 mL/min,进样量为10
µL,柱温为30 ℃,检测波长分别为283、330、520、220 nm。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SPSS 26.0、SIMCA 14.1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~
0.166 mg/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。
关键词 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
Content determination and chemical pattern recognition analysis of Biantong capsules
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SHU Bo ,LEI Guoping ,YUAN Bin(1. Dept. of Pharmacy,the Affiliated Hospital of North Sichuan Medical
College, Sichuan Nanchong 637000, China;2. Nanchong Institute for Food and Drug Control, Sichuan
Nanchong 637000,China;3. Institute of Materia Medica,North Sichuan Medical College,Sichuan Nanchong
637000,China)
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 C18 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 S11-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,
Δ 基金项目 四川省科技计划项目(No.2020YFS0528);南充市科 naringin,neohesperidin,echinacoside and verbascoside were
技项目(市校科技战略合作专项)(No.19SXHZ0450)
all greater than 1. CONCLUSIONS The method for
*第一作者 副主任中药师。研究方向:临床合理用药、中药质量。
电话:0817-2801702。E-mail:30387948@qq.com simultaneous determination of 11 components in Biantong
# 通信作者 副研究员,硕士。研究方向:天然产物药效评价。电 capsules, including narirutin, is successfully established.
话:0817-3373323。E-mail:sjqp00@163.com Combined with chemical pattern recognition analysis,it can be
中国药房 2022年第33卷第18期 China Pharmacy 2022 Vol. 33 No. 18 ·2209·