骨刺消痛胶囊HPLC特征图谱及多成分含量测定研究  

Study on HPLC characteristic chromatogram and multi-component determination of Guci Xiaotong capsules

作　　者：穴卓 笔雪艳 林林 XUE Zhuo;BI Xue-yan;LIN Lin(Heilongjiang Institute for Drug Control,Harbin 150088,China)

机构地区：[1]黑龙江省药品检验研究中心,哈尔滨150088

出　　处：《药物分析杂志》2020年第2期295-303,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：2017年国家评价性抽验项目。

摘　　要：目的:建立骨刺消痛胶囊的HPLC特征图谱,并对其5个主要成分(龙胆苦苷、甘草苷、丹皮酚、欧前胡素、异欧前胡素)进行含量测定,通过对不同企业骨刺消痛胶囊的研究,建立全面而统一的质量控制方法。方法:采用C18色谱柱(4.6 mm×250 mm,5μm),以乙腈(A)-水(B)为流动相进行梯度洗脱,流速1.0 mL·min-1,柱温为25℃,检测波长为274 nm(1~40 min,龙胆苦苷、甘草苷、丹皮酚)和254 nm(40.01~70 min,欧前胡素、异欧前胡素)。建立骨刺消痛胶囊HPLC特征图谱,同时测定5个主要成分的含量。结果:通过对21个厂家骨刺消痛胶囊的HPLC特征图谱进行研究,确定了12个共有峰,经过归属验证,指认其中6个特征成分,分别为龙胆苦苷(4号峰)、甘草苷(5号峰)、丹皮酚(7号峰)、欧前胡素(8号峰)、蒿本内酯(9号峰)、异欧前胡素(12号峰)。利用相似度评价软件对各批次样品特征图谱进行分析,相似度均在0.90以上。在建立的色谱条件下对其中5个主要成分进行测定,各组分间分离度良好,方法精密度和重复性RSD均<2.0%,供试品溶液在24 h内稳定,龙胆苦苷、甘草苷、丹皮酚、欧前胡素、异欧前胡素进样量分别在0.110 1~1.101、0.007 2~0.071 8、0.074 9~0.748 7、0.007 7~0.076 6、0.003 0~0.030 1μg范围内线性关系良好,加样回收率分别为103.4%、87.6%、84.7%、94.6%和96.3%。20批骨刺消痛胶囊中上述5个成分的含量分别为1.322~2.453、0.032~0.222、1.208~1.572、0.052~0.313和0.028~0.109 mg·g-1。结论:所建立的骨刺消痛胶囊HPLC特征图谱和定量测定分析方法可全面有效地评价该制剂的质量。Objective:To establishan HPLC characteristic chromatogram of Guci Xiaotong capsules and determine five components(gentiopicroside,liquiritin,paeonol,imperatorin and isoimperatorin).To provide a comprehensive and unified quality control method based on analysis of samples from different enterprises. Methods:The analysis was performed on a C18 column(4.6 mm ×250 mm,5 μm)with gradient elution of acetonitrile(A)-water(B)at a flow rate of 1.0 ml·min-1. The column temperature was 25 ℃. The detection wavelength were 274 nm for gentiopicroside,liquiritin and paeonol(1-40 min)and 254 nm for imperatorin and isoimperatorin(40.01-70 min). The HPLC characteristic chromatogram of Guci Capsule was established and the five components were determined. Results:Through the study on HPLC characteristic chromatograms of 21 manufacturers samples,12 common peaks were designated and 6 of which were identified as gentiopicroside(peak 4),liquiritin(peak 5),paeonol(peak 7),imperatorin(peak 8),ligustilide(peak 9)and isoimperatorin(peak 12)by comparison with the reference substances. The similarities of samples were over 0.99. Under the established chromatographic conditions,the five main components were separated well. The RSD values of precision and repeatability were all less than 2.0% and the test solution was stable in 24 hours. The linear ranges of gentiopicroside,liquiritin,paeonol,imperatorin and isoimperatorin were 0.110 1-1.101,0.007 2-0.071 8,0.074 9-0.748 7,0.007 7-0.076 6 and 0.003 0-0.030 1 μg,respectively. The recoveries were 103.4%,87.6%,84.7%,94.6% and 96.3% respectively. The contents of the above mentioned five components were 1.322-2.453,0.032-0.222,1.208-1.572,0.052-0.313 and 0.028-0.109 mg·g-1. Conclusion:The established HPLC characteristic chromatograms and quantitative analysis methods offered comprehensive and effective evaluation approach for quality control of the Guci Xiaotong capsules.

关 键 词：骨刺消痛胶囊 特征图谱 多指标含量测定 龙胆苦苷 甘草苷 丹皮酚 欧前胡素 异欧前胡素 蒿本内酯 质量控制 

分 类 号：R917[医药卫生—药物分析学]