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高效液相色谱一测多评法评价乳核散结片10种成分质量

Simultaneous Determination of Ten Constituents in Ruhe Sanjie Tablet by HPLC-QAMS

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【作者】 薛艳丽娄朝晅薛小琦田广林

【Author】 XUE Yanli;LOU Zhaoxuan;XUE Xiaoqi;TIAN Guanglin;Department of Pharmacy,the First Affiliated Hospital of Henan University of Science and Technology;Forensic Experiment Teaching Center,Henan University of Science and Technology;Suicheng Pharmaceutical Co.,Ltd;

【通讯作者】 娄朝晅;

【机构】 河南科技大学第一附属医院药学部河南科技大学法医学实验教学中心遂成药业股份有限公司

【摘要】 目的 建立高效液相色谱一测多评法评价乳核散结片中洋川芎内酯I、洋川芎内酯H、阿魏酸松柏酯、藁本内酯、欧当归内酯A、淫羊藿苷、宝藿苷I、双去甲氧基姜黄素、去甲氧基姜黄素及姜黄素质量。方法 乳核散结片70%甲醇提取物的分析采用Agilent TC-C18色谱柱(4.6 mm×250 mm, 5μm),流动相乙腈-0.6%醋酸溶液,梯度洗脱,流速1.0 mL·min-1,检测波长280 nm(检测洋川芎内酯I、洋川芎内酯H、阿魏酸松柏酯、藁本内酯、欧当归内酯A、淫羊藿苷和宝藿苷I)和420 nm(检测双去甲氧基姜黄素、去甲氧基姜黄素和姜黄素),柱温30℃。内参物为淫羊藿苷,建立其他9种成分的相对校正因子,计算各成分含量。结果 10种成分浓度分别在0.99~39.60μg·mL-1(r=0.999 7),0.56~22.40μg·mL-1(r=0.999 5),28.82~1152.80μg·mL-1(r=0.999 8),20.78~831.20μg·mL-1(r=0.999 5),3.19~127.60μg·mL-1(r=0.999 7),24.76~990.40μg·mL-1(r=0.999 8),13.67~546.80μg·mL-1(r=0.999 6),3.99~159.60μg·mL-1(r=0.999 4),5.36~214.40μg·mL-1(r=0.999 8)和9.93~397.20μg·mL-1(r=0.999 9)范围内有良好线性关系,平均加样回收率(RSD)分别为97.85%(0.82%),96.97%(1.03%),100.07%(0.62%),99.42%(1.34%),98.64%(0.80%),99.43%(1.13%),100.02%(0.67%),98.35%(0.97%),98.70%(1.23%)和97.99%(1.65%),外标法实测结果与一测多评法计算结果差异无统计学意义。结论 该实验建立的高效液相色谱一测多评法可靠,简便,灵敏,符合方法学验证要求,可用于乳核散结片质量控制。

【Abstract】 Objective To establish a method for the application of high-performance liquid chromatography combined with quantitative analysis of multi-components by single-marker(HPLC-QAMS) technology in the quality evaluation of senkyunolide I,senkyunolide H,coniferyl ferulate, ligustilide, levistilide A,icariin, baohuosideⅠ,bisdemethoxycurcumin, demethoxycurcumin and curcumin in Ruhe Sanjie tablets. Methods Agilent TC-C18 chromatographic column(4.6 mm×250 mm, 5 μm) was used to analyze of 70% methanol extract of Ruhe Sanjie tablets.The mobile phase was acetonitrile-0.6% acetic acid solution with gradient elution at a flow rate of 1.0 mL·min-1.The detection wavelength were set at 280 nm for senkyunolide I,senkyunolide H,coniferyl ferulate, ligustilide, levistilide A,icariin and baohuosideⅠ,and 420 nm for bisdemethoxycurcumin, demethoxycurcumin and curcumin.The column temperature was 30 ℃.Using icariin as an internal standard, the relative correction factors of the other nine constituents were calculated, after which the content determination was made. Results Ten components showed good linear relationships within the ranges of 0.99-39.60 μg·mL-1(r=0.999 7),0.56-22.40 μg·mL-1(r=0.999 5),28.82-1152.80 μg·mL-1(r=0.999 8),20.78-831.20 μg·mL-1(r=0.999 5),3.19-127.60 μg·mL-1(r=0.999 7),24.76-990.40 μg·mL-1(r=0.999 8),13.67-546.80 μg·mL-1(r=0.999 6),3.99-159.60 μg·mL-1(r=0.999 4),5.36-214.40 μg·mL-1(r=0.999 8),and 9.93-397.20 μg·mL-1(r=0.999 9),respectively.And the average recoveries(RSDs) of each components were 97.85%(0.82%),96.97%(1.03%),100.07%(0.62%),99.42%(1.34%),98.64%(0.80%),99.43%(1.13%),100.02%(0.67%),98.35%(0.97%),98.70%(1.23%) and 97.99%(1.65%),respectively.There was no difference between the measured results of external standard method(ESM) and the calculated results of one measurement and multiple evaluation method. Conclusion The established method is reliable, simple and sensitive, which meets the requirements of methodology verification. It can be used for the quality control of Ruhe Sanjie tablets.

【基金】 河南省重大科技专项(创新示范专项)(191110311100)
  • 【文献出处】 医药导报 ,Herald of Medicine , 编辑部邮箱 ,2022年11期
  • 【分类号】R286.0
  • 【下载频次】66
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