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目的:建立沉香化气丸的超高效液相色谱(UPLC)指纹图谱,为评价该制剂的整体质量提供参考依据。方法:采用Phenomenex Kinetex C_(18)色谱柱(4.6 mm×100 mm,2.7μm),流动相乙腈(A)-0.1%磷酸水溶液(B)梯度洗脱(0~7 min,12%~16%A;7~14 min,16%~19%A;14~16 min,19%~25%A;16~19 min,25%~28%A;19~22 min,28%~42%A;22~27 min,42%~46%A;27~33 min,46%~48%A;33~37 min,48%~72%A;37~39 min,72%~90%A;39~42 min,90%A),分段变波长测定(0~3 min,285 nm;3~20 min,210 nm;20~24 min,254 nm;24~42 min,210 nm),进样量2μL,流速调整至0.8 mL·min~(-1);根据相似度评价,结合化学计量学方法对沉香化气丸进行质量评价。结果:建立了20批沉香化气丸的UPLC指纹图谱,标定了27个共有峰,通过对照品指认了12个共有峰,20批样品指纹图谱的相似度均>0.98。通过聚类分析可将样品聚为3类,结合主成分分析、正交偏最小二乘法-判别分析发现7个成分是造成不同批次样品差异性的主要标记物。结论:指纹图谱的构建与化学模式识别可为沉香化气丸的质量控制提供更为全面的信息参考。建立的UPLC指纹图谱方法稳定可行。
OBJECTIVE: To establish the UPLC fingerprint of Shen Xiang Qi Qi Wan, and provide a reference for evaluating the overall quality of the preparation. METHODS: The mobile phase was eluted with a gradient of acetonitrile (A) - 0.1% phosphoric acid in water (B) over a Phenomenex Kinetex C 18 column (4.6 mm × 100 mm, 2.7 μm) A, 7-14 min, 16-19% A, 14-16 min, 19-25% A, 16-19 min, 25-28% A, 19-22 min, 28% -42% A, 22- 27 min, 42% -46% A; 27-33 min, 46- 48% A; 33-37 min, 48-72% A; 37-39 min, 72-90% 42 min, 90% A), and the variation of the wavelength was determined by sub-sampling (0-3 min, 285 nm; 3-20 min, 210 nm; 20-24 min, 254 nm; 24-42 min, 210 nm) 2μL, the flow rate was adjusted to 0.8mL · min ~ (-1); According to the similarity evaluation, combined with chemometrics method to evaluate the quality of Shen Xiang Hua Qi Wan. Results: UPLC fingerprints of 20 batches of aloe vera pills were established, 27 common peaks were calibrated, and 12 common peaks were identified by reference substance. The fingerprint similarity of 20 batches of samples was> 0.98. By cluster analysis, the samples can be grouped into three categories. Combined with principal component analysis and orthogonal partial least square method - discriminant analysis, seven components were found to be the main markers for the differences of samples from different batches. Conclusion: The construction of fingerprint and chemical pattern recognition can provide a more comprehensive information reference for the quality control of Shen Xiang Qi Qiu Pills. The established UPLC fingerprinting method is stable and feasible.