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中国医药导刊 ›› 2021, Vol. 23 ›› Issue (4): 272-276.

• 检验检测 • 上一篇    下一篇

HPLC法同时测定清络通脉片中7种成分的含量

纪世彬, 赵万隆*   

  1. 上海市青浦食品药品检验所检验室, 上海 201799
  • 收稿日期:2020-11-12 修回日期:2021-05-19 出版日期:2021-04-28 发布日期:2021-04-28

Simultaneous Determination of 7 Kinds of Components in Qingluo Tongmai Tablets by HPLC

 JI Shibin, ZHAO Wanlong*   

  1. Testing Laboratory, Shanghai Qingpu Institute for Food and Drug Control, Shanghai 201799, China
  • Received:2020-11-12 Revised:2021-05-19 Online:2021-04-28 Published:2021-04-28

摘要: 目的: 建立同时测定清络通脉片中7种成分含量的HPLC方法,旨在为提高清络通脉片质量标准提供科学依据。方法: 以芍药苷、丹皮酚、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚制备对照品溶液,以不同批次的清络通脉片制备供试品溶液,以缺赤芍、牡丹皮和大黄的阴性样品制备阴性对照溶液,采用C18色谱柱(4.6 mm×250 mm,5 μm),0.1%磷酸溶液和乙腈分别作为流动相A和流动相B,进行梯度洗脱,流速为1.0 mL·min-1、检测波长为230 nm、柱温30 ℃,进样量20 μL。结果: 芍药苷、丹皮酚、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚各峰之间分离度良好,且分别在9.90~138.54、0.53~7.39、0.99~13.80、2.01~28.17、2.01~28.13、3.01~42.08、0.81~11.29 μg·mL-1的范围内线性关系良好;精密度与重复性RSD均<2.0%;供试品溶液在12 h内稳定性较好;7种成分的平均回收率均大于97%,RSD <2.0%。结论: 该方法在清络通脉片的质量评价中应用效果明显,操作简便,该制剂各组分分离度好,结果准确、可靠,可作为提高清络通脉片质量标准的依据。
    

关键词: font-size:medium, ">清络通脉片;高效液相色谱法;含量测定;芍药苷;丹皮酚;芦荟大黄素 ,

Abstract: Objecetive: To develop a reliable HPLC method for the simultaneous determination of 7 components in qingluo tongmai tablets,to provide scientific basis for improving the quality standard of qingluo tongmai tablets. Methods: Paeoniflorin, paeonol, aloe emodin, rhein, emodin, chrysophanol, emodin methyl ether were used to make reference substance.Different batches of qingluo tongmai tablets were used to make test products.The negative samples without radix paeoniae rubra, cortex moutan and rhubarb were used as negative control.Using the C18 chromatographic column(4.6 mm×250 mm,5 μm), 0.1% phosphoric acid solution and acetonitrile as mobile phases, denoted as A and B respectively, using a gradient ratio of mobile phase A and B for elution, and detection at 1.0 mL·min-1, 230 nm, and 30°C. The injection volume is 20 μL. Results:The paeoniflorin, paeonol, aloe emodin,rhein,emodin, chrysophanol and physcion were well separated and showed good linear relationship within the ranges of 9.90-138.54,0.53-7.39,0.99-13.80,2.01-28.17,2.01-28.13,3.01-42.08,0.81-11.29 μg·mL-1, respectively. The precision and repeatability RSD were all less than 2.0%. The stability of the sample solution was good within 12 h. The average recovery was greater than 97%, and RSD was less than 2.0%. Conclusion: The method has obvious application effect in the quality evaluation of qingluo tongmai tablets, with simple operation, good separation of the components of the preparation, accurate and reliable results, and can be used as a basis for improving the quality standard of qingluo tongmai tablets.
  

Key words: font-size:medium, ">Qingluo tongmai tablets; HPLC; Content determination; Paeoniflorin; Paeonol; Aloe emodin

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