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中国药物评价 ›› 2020, Vol. 37 ›› Issue (3): 196-200.

• 评价技术与方法 • 上一篇    下一篇

固相萃取技术-HPLC法同时测定滑膜炎片/颗粒中防己诺林碱和粉防己碱的含量

康凯1, 张静娇1, 刘斯亮1, 李娜2   

  1. 1.大连市检验检测认证技术服务中心 辽宁 大连 116021;
    2.辽宁中医药大学 辽宁 大连 116600
  • 收稿日期:2019-12-11 修回日期:2020-01-13 出版日期:2020-06-28 发布日期:2020-07-15
  • 基金资助:
    2019年国家药品评价性抽验项目

Simultaneous Determination of Tetrandrine and Fangchinoline in HuamoyanTablets/Granules by Solid Phase Extraction-HPLC Method

  1. 1.Dalian Inspection and Certification Technical Service Center, Liaoning Dalian 116021, China;
    2.Liaoning University of Chinese Medicine, Liaoning Dalian 116600, China
  • Received:2019-12-11 Revised:2020-01-13 Online:2020-06-28 Published:2020-07-15

摘要: 目的:建立滑膜炎片/颗粒中防己诺林碱和粉防己碱的含量测定方法。方法:对固相萃取条件进行了研究,最终选择以0.1mol·L-1盐酸溶液、甲醇为清洗溶液,以新制的乙腈-浓氨试液(95∶5)混合溶液为洗脱溶液,基本消除了干扰成分对测定的影响,色谱图背景吸收小,基线稳定;采用SePax HP-C18(4.6×150 mm,5 μm)色谱柱;流动相:甲醇-0.1%三乙胺(78∶22);流速:1.0 mL·min-1;检测波长为280 nm;柱温:35 ℃。结果:防己诺林碱浓度在2.50~24.99 μg·mL-1 (r=0.999 9)范围、粉防己碱浓度在5.10~50.99 μg·mL-1(r=0.999 9)范围与峰面积呈良好的线性关系;平均加样回收率:防己诺林碱99.7%(n=6)、粉防己碱100.3%(n=6)。结论:本方法简便、准确,适用于滑膜炎片/颗粒的质量控制。

关键词: font-size:medium, ">固相萃取;高效液相色谱法;滑膜炎片/颗粒;防己诺林碱;粉防己碱;SPSS

Abstract: Objective: To establish a method for thedeterminationof tetrandrine and fangchinoline in Huamoyantablets/granules.Methods: Toestablishthe conditions ofsolid-phase extraction. Finally, a 0.1 mol·L-1 hydrochloric acid solution and methanol were selected as the cleaning solution, and a newly prepared acetonitrile-strongammonia solution (95∶5) was used as the eluent, which was basically eliminatedthe influence of interference components on the measurement, the background absorption of the chromatogram is small, and the baseline is stable; a SePax HP-C18 (4.6×150 mm, 5 μm) column is used; mobile phase: methanol-0.1% triethylamine (78∶22); flow rate: 1.0 mL·min-1; detection wavelength is 280 nm; column temperature: 35 ℃. Results: The concentration of tetrandrine in the range of 2.50~24.99μg·mL-1 (r=0.999 9), the concentration of fangchinoline in the range of 5.10~50.99 μg·mL-1 (r=0.999 9) showed a good linear relationship with the peak area; the average ratesofrecovery:99.7% of tetrandrine(n=6) and100.3% of fangchinoline(n=6). Conclusion: This method is simple, accurate and suitable for the quality control of Huamoyan tablets/ granules.

Key words: font-size:medium, ">Solid-phase extraction; HPLC; Huamoyan tablets/granules; Tetrandrine; Fangchinoline; SPSS

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