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高效液相色谱法同时测定黄芪精颗粒中3种黄酮类成分及其指纹图谱研究
Simultaneous determination of 3 flavonoids in Huangqijing granules by HPLC and their fingerprints
【摘要】 目的建立HPLC同时测定黄芪精颗粒中3种黄酮类成分的含量,并对其进行指纹图谱研究。方法采用Agilent高效液相色谱仪,5 HC C18(2)色谱柱(4.6 mm×250 mm,5μm),VWD检测器,流速1.0 mL·min-1,进样量10μL,柱温25℃,毛蕊异黄酮苷、毛蕊异黄酮、芒柄花素的含量测定和指纹图谱分别采用不同梯度条件进行洗脱,3个成分含量测定的检测波长为260 nm,指纹图谱的检测波长为240 nm。结果毛蕊异黄酮苷、毛蕊异黄酮、芒柄花素分别在0.0257~1.0280、0.039 95~1.5980、0.0110~0.4400μg内与峰面积线性关系良好,平均加样回收率分别为104.3%、97.8%、96.9%,RSD值均小于3%。11批黄芪精颗粒样品的指纹图谱相似度均大于0.9,标定10个共有成分峰,确认毛蕊异黄酮苷、芒柄花苷、毛蕊异黄酮、芒柄花素4个成分。结论黄芪精颗粒中3个黄酮类成分的含量测定方法及HPLC指纹图谱方法简便、稳定、可靠,可为黄芪精颗粒的质量控制提供参考。
【Abstract】 Objective To determine the content of 3 flavonoids in Huangqijing granules by HPLC and their fingerprints. Methods Agilent 5 HC C18(2) column(4.6 mm×250 mm, 5 μm) was used for separation and the VWD detector was used. The flow rate, injection volume and column temperature were 1.0 mL·min-1, 10μL, and 25℃, respectively. The gradient elution was performed by the different mobile phases to determine the calycosin-7-O-β-D-glucoside, calycosin and formononetin and their fingerprints. The detection wavelength of the 3 components was 260 nm and the detection wavelength of the fingerprint was 240 nm. Results Calycosin-7-O-β-D-glucoside, calycosin and formononetin showed good linearity at 0.0257-1.0280 μg, 0.039 95-1.5980 μg, and 0.0110-0.4400 μg, respectively, with average recoveries of 104.3%, 97.8% and 96.9%,respectively, and RSD all less than 3%. The similarity of the 11 batches of samples was greater than 0.9. Ten common peaks were found in the fingerprints of 11 batches of samples. Four components(calycosin-7-O-β-D-glucoside, ononin, calycosin and formononetin) were confirmed. Conclusion The determination method and HPLC fingerprint method of Huangqijing granules are simple, stable and reliable. Combining with the original quality standard of astragaloside Ⅳ quality control method, the quality of Huangqijing granules can be comprehensively evaluated and can provide reference for the quality control.
【Key words】 Huangqijing granule; fingerprint; HPLC; calycosin-7-O-β-D-glucoside; ononin; calycosin; formononetin;
- 【文献出处】 中南药学 ,Central South Pharmacy , 编辑部邮箱 ,2019年04期
- 【分类号】R286.0;O657.72
- 【被引频次】10
- 【下载频次】560