基于UPLC指纹图谱和多成分含量测定的解郁丸质量评价研究

Quality evaluation of Jieyu pills based on UPLC fingerprint and muti-component content determination

关键词:  解郁丸  超高效液相色谱  指纹图谱  多成分含量测定  质量评价

Key words:  Jieyu pills  UPLC  fingerprint  content determination  quality evaluation.

摘要:

目的：建立解郁丸的超高效液相色谱(UPLC)指纹图谱及多成分含量测定方法，为解郁丸科学全面的质量控制和评价提供参考。方法：采用UPLC法，色谱柱为Accucore aQ(2.1 mm×150 mm,2.6 μm)，流动相为水(A)和乙腈(B)，梯度洗脱，体积流量为0.2 mL·min-1，柱温30 ℃，检测波长205 nm、240 nm。结果：建立了10批解郁丸的指纹图谱，在205 nm下共标定出51个共有峰,在240 nm下共标定出31个共有峰,相似度均在0.930以上,经对照品比对指认出柴胡皂苷F、柴胡皂苷A、柴胡皂苷D、甘草查尔酮A、蒿本内酯、莪术醇、芍药内酯苷、芍药苷、甘草苷、芦丁、洋川芎内酯H、茯苓酸A 12个成分，主成分分析结果显示12个成分均与样品相关性较强；进一步建立了12个成分的含量测定方法,其在各自浓度范围内线性关系良好(r≥0.9990)，精密度、重复性、稳定性试验结果均良好，平均加样回收率分别为98.18%~101.31%，RSD为1.66%～2.87%，含量分别为0.3242~0.5106、0.7235~1.1311、0.3884~0.6028、0.0051~0.0065、0.6953~0.9856、0.1975~0.2375、1.6459~2.1189、1.8675~2.8654、0.1336~0.1769、0.1868~0.2197、0.2754~0.3065、0.0254~0.0337 mg·g-1。结论：本研究所建立的解郁丸指纹图谱和12个成分含量测定方法准确、稳定、可行，为全面控制和评价解郁丸的质量提供科学依据。

Abstract:

OBJECTIVE: To establish the fingerprint and multi-component content determination method of Jieyu pills based on ultra performance liquid chromatography (UPLC), to provide reference for its scientific and comprehensive quality control and evaluation. METHODS: The separation was performed on an Accucore aQ(2.1 mm×150 mm,2.6 μm) with water (A) and acetonitrile (B) gradient elution as the mobile phase by UPLC. The volume flow rate was 0.2 mL·min-1, the column temperature was 30℃, the detection wavelengths were 205 nm and 240 nm. RESULTS: The UPLC fingerprint of 10 batches of Jieyu pills was established, 51 common peaks were calibrated at 205nm and 31 common peaks were calibrated at 240 nm. The similarities were greater than 0.930. Twelve chromatographic peaks including saikosaponin F, saikosaponin A, saikosaponin D, licochalcone A, ligustilide, curcumol, albiflorin, paeoniflorin, liquiritin, rutin, senkyunolide H, and poricoic acid A were identified with reference substances. The results of principal component analysis showed that these 12 components have a strong correlation with Jieyu pills. The content determination method of 12 components was further established. 12 components showed good linear relationships within their respective concentration ranges (r≥0.9990) with good precision, repeatability, and stability test results. The average recoveries were 98.18%-101.31%, with RSDs of 1.66%-2.87%, the contents were 0.3242-0.5106, 0.7235-1.1311, 0.3884-0.6028, 0.0051-0.0065, 0.6953-0.9856, 0.1975-0.2375, 1.6459-2.1189, 1.8675-2.8654, 0.1336-0.1769, 0.1868-0.2197, 0.2754-0.3065, 0.0254-0.0337 mg·g-1. CONCLUSION: The method of fingerprint and content determination of 12 components established in this study is accurate, stable, and feasible, which can provide a scientific basis for comprehensive control and evaluation of the quality of Jieyu pills.