十味鹅黄颗粒HPLC指纹图谱及8种主要成分含量测定

目的：采用高效液相色谱（HPLC）法，研究建立十味鹅黄颗粒指纹图谱定性和8种主要成分定量分析的测定方法，为十味鹅黄颗粒的质量控制提供更为可靠的方法和依据。方法：色谱柱为ZORBAX Eclipse XDB-C₁₈（4.6 mm×250 mm，5 μm）；以乙腈-水为流动相，梯度洗脱，流速为1.0 mL·min^-1，柱温为30℃，检测波长为230 nm。结果：含量测定结果显示，十味鹅黄颗粒中的主要成分芍药苷、升麻素苷、毛蕊异黄酮葡萄糖苷、升麻素、5-O-甲基维斯阿米醇苷、毛蕊异黄酮、丹皮酚和木兰脂素8个成分的含量范围分别为0.386 8~0.448 5，0.132 7~0.149 1，0.122 3~0.135 7，0.023 0~0.029 6，0.247 6~0.275 5，0.037 2~0.051 4，0.122 7~0.153 7，0.4492~0.536 0 mg·g^-1；方法学考察结果显示各项指标符合含量测定要求；10批次十味鹅黄颗粒样品的指纹图谱与其指纹图谱共有模式相比较相似度均大于0.9，标定了共有峰11个，并对其中8个共有指纹峰进行了指认和归属。结论：所建立的指纹图谱共有模式特征性强，多指标成分含量测定同时结合指纹图谱分析能更为全面地对十味鹅黄颗粒的质量进行控制。

HPLC fingerprint and determination of eight main components of Shiweiehuang granules

OBJECTIVE To establish a method for the qualitative analysis of fingerprints and quantitative analysis of eight main components of Shiweiehuang granules by HPLC, and to provide a more reliable method and basis for the quality control of Shiweiehuang granules. METHODS The chromatographic column was a ZORBAX Eclipse XDB-C₁₈ (4.6 mm×250 mm, 5 μm); acetonitrile-water was used as the mobile phase with gradient elution at a flow rate of 1.0 mL·min^-1, the column temperature was 30℃, and the detection wavelength was 230 nm. RESULTS The result of determination showed that the content of Paeoniflorin, Prim-O-glucosylcimifugin, Calycosin-7-glucoside, Cimifugin, 5-O-methylvisammioside, Calycosin, Paeonol and Magnolin were 0.386 8-0.448 5,0.132 7-0.149 1,0.122 3-0.135 7,0.023 0-0.029 6, 0.247 6-0.275 5,0.037 2-0.051 4,0.122 7-0.153 7,0.449 2-0.536 0 mg·g^-1, respectively. The result of methodological study showed that all the indexes met the requirements for content determination. Compared with the common pattern of fingerprints, the similarities of 10 batches of samples were greater than 0.9 with 11 common peaks, 8 of which were identified and assigned CONCLUSION The common pattern of fingerprints is well characterized. The better quality control of Shiweiehuang granules can be achieved by multi-index composition determination combined with fingerprint analysis