目的 建立安宫牛黄丸特征图谱分析方法，以全面整体表征安宫牛黄丸质量属性和特性，并应用于10批次安宫牛黄丸成品质量检测分析。方法 采用UPLC-PDA多波长分析方法，Waters Cortecs Shield RP₁₈（100 mm×2.1 mm，1.6 μm）色谱柱，流动相乙腈-0.3%磷酸水溶液，梯度洗脱，体积流量0.2 mL/min，柱温38℃，检测波长240、262、274、330、360、440 nm。结果 所建立特征图谱分析方法稳定可行，分析指认了安宫牛黄丸成品中35个特征峰，其中包括可鉴别原料药材天然属性的天然麝香特征峰（峰6）、天然牛黄特征峰（峰33），并同时测定了其中13个指标性成分（栀子苷、京尼平龙胆双糖苷、西红花苷I、西红花苷Ⅱ、盐酸小檗碱、盐酸黄连碱、盐酸巴马汀、表小檗碱、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、姜黄素）含量，10批次安宫牛黄丸中13个指标性成分质量分数均值依次为2.87、1.14、0.40、0.03、3.17、0.94、0.74、0.58、10.01、1.62、0.34、0.17、0.05 mg/g，RSD为4.19%~20.81%，10批次安宫牛黄丸均可稳定检出35个特征峰，其中天然麝香、天然牛黄特征峰相对峰面积均值分别为0.031、0.003，各特征峰相对峰面积的RSD为1.5%~26.79%。结论 特征图谱分析表明，10批次安宫牛黄丸成品质量相对稳定，均显示了天然麝香、天然牛黄、黄丝郁金原料药材的特异性质量表征；指标性成分含量分析表明，10批次样品中指标性成分含量波动较大的主要源于黄芩和黄丝郁金药材，栀子药材中西红花苷I含量和黄连药材中4个生物碱成分含量较为稳定。

Objective To establish an Angong Niuhuang Pills (ANP) characteristic spectrum analysis method, and to comprehensively characterize the quality properties and characteristics of ANP, and then to apply it to the quality detection and analysis of 10 batches of ANP, and to find out the specificity of the quality characterization of ANP. Methods The UPLC-PDA multi-wavelength was used in the method, and a Waters Cortecs shields RP₁₈ Column (100 mm×2.1 mm, 1.6 μm) was used, the mobile phase was acetonitrile and 0.3% phosphoric acid solution, the detection wavelength was set at 240, 262, 330, 360, 274, and 440 nm, the column temperature was kept at 38℃, and the flow rate was 0.2 mL/min. Results The results showed that the established analytical method can simultaneously determine 13 index components (including geniposide, genipin1-gentiobioside, crocin I, crocin Ⅱ, berberine hydrochloride, coptis hydrochloride, palmatine chloride, epiberberine, baicalin, wogonoside, baicalein, wogonin and curcumin) in ANP, and a total of 35 characterstic peaks were identified in ANP. It included natural musk characteristic peak and natural bovis calculus characteristic peak which can identify the natural properties of raw materials. The mean values of the 13 index components in 10 batches of ANP were 2.87, 1.14, 0.40, 0.03, 3.17, 0.94, 0.74, 0.58, 10.01, 1.62, 0.34, 0.17, 0.05 mg/g, respectively. The RSD values ranged from 4.19% to 20.81%. All the 10 batches of ANP could be detected with 35 characteristic peaks, the average area values of natural musk and natural bovis calculus characteristic peaks were 0.031 and 0.003, and the RSD values ranged from 1.5% to 26.79%. Conclusion According to the analysis of characteristic spectrum, the quality of finished products of 10 batches of ANP was relatively stable, and all showed the specific quality characterization of raw materials of natural musk, natural bovis calculus and Curcumae Radix; According to the analysis of the content of index components, the large fluctuation of the index components in 10 batches of samples mainly comes from Scutellaria baicalensis and Curcumae Radix, while the content of crocin I in Gardeniae Fructus and four alkaloids in Coptidis Rhizoma were relatively stable.

R286.02

国家中医药标准化项目：安宫牛黄丸标准化建设（ZYB2H-C-BJ-03）