目的 建立戊己丸UPLC-MS/MS指纹图谱分析方法,确定各色谱峰的药材来源,同时对各成分进行定性研究,为其物质基础、质量控制、研究开发和应用提供科学依据。方法 采用Acquity UPLC BEH C₁₈色谱柱(100 mm×2.1 mm,1.7μm),以0.05%甲酸水溶液-乙腈为流动相,梯度洗脱;柱温40℃,体积流量0.4 mL/min,进样量2μL。利用"中药色谱指纹图谱相似度评价系统2004A版"对其进行相似度评价。结果 建立了戊己丸UPLC-MS/MS指纹图谱的共有模式,确定了38个共有峰,并根据对照品和参考文献定性指认了9个共有峰分别为盐酸小檗碱、盐酸巴马汀、盐酸药根碱、黄连碱、表小檗碱、吴茱萸碱、吴茱萸次碱、吴茱萸内酯、芍药苷,推断出4个共有峰分别为木兰花碱、芍药内酯苷、格陵兰黄连碱、1-甲基-2-壬基-4(1H)-喹诺酮。对11批由不同产地和品种药材制备的戊己丸的相似度进行了考察,其相似度在0.90以上。结论 建立了戊己丸的UPLC-MS/MS指纹图谱分析方法,该分析方法快速、灵敏、简便,为戊己丸的质量控制提供实验依据。

Objective To establish and study the UPLC-MS/MS fingerprint, to ascertain the medicinal source of chromatographic peaks, and to identify the chemical constituents for providing scientific basis in effective substance foundation and quality control of Wuji Pill. Methods The fingerprint of Wuji Pill was developed with ultra-performance liquid chromatography (UPLC), and the Acquity UPLC BEH C₁₈ column (100 mm×2.1 mm, 1.7 μm) was used in the gradient elution with a mobile phase of acetonitrile-water (0.05% formic acid):The flow rate was 0.4 mL/min, the column temperature was 40℃. Similarity evaluation was used to evaluate the quality of herbs from different areas. Results The fingerprint of Wuji Pill was established with good precision, reproducibility, and stability obtaining within 55 min, and 38 peaks in the fingerprint were designed. Twenty samples could be classified into two clusters. According to the reference, and qualitative and references identified a total of nine peaks were berberine, palmatine, jatrorrhizine, coptisine, epiberberine, evodiamine, rutaecarpine, evodine, and paeoniflorin inferred that the four common peaks were magnolia base magnoflorine, albiflorin, theophylline, and methyl-2-nonyl-4(1H)-quinolone. Conclusion The establishment of UPLC fingerprint of Wuji Pill and application of chemical pattern recognition can provide a more comprehensive reference for the quality control of herbs.

国家自然科学基金资助项目(81460609)