HPLC-DAD波长切换法建立加味三妙丸的指纹图谱

目的：建立加味三妙丸的多波长切换HPLC指纹图谱，并对共有峰进行归属，用于评价其质量。方法：采用HPLC-DAD梯度洗脱波长切换法，使用Ultimate AQ-C₁₈（4.6 mm×250 mm，5 μm）色谱柱，以0.1%三乙胺水1 000 mL+冰醋酸0.44 mL为流动相A，乙腈为流动相B，梯度洗脱，流速1 mL·min^-1，检测波长为291 nm（0～60 min，黄柏碱）、243 nm（60～70 min，落新妇苷、杯苋甾酮）、378 nm（70～80 min，小檗碱）、336 nm（80～120 min），柱温30℃，进样量10 μL。采用中药色谱指纹图谱相似度评价系统软件（2004A版）处理11个样品色谱图。结果：建立加味三妙丸指纹图谱，标记18个共有峰。对共有峰进行成分及各药材归属，并指认出黄柏碱、落新妇苷、杯苋甾酮、小檗碱4个成分。结论：建立的指纹图谱能有效全面地评价加味三妙丸的质量。

Objective: To establish fingerprint of modified Sanmiao pills by HPLC-DAD wavelength switching, and identify the characteristic peaks for quality evaluation.Methods: HPLC-DAD and the gradient elution wavelength shifts technique were adopted for the study.The column was an Ultimate AQ-C₁₈(4.6 mm×250 mm, 5 μm) column with gradient elution at a flow rate of 1 mL·min^-1;the mobile phase A was 1 000 mL of 0.1% triethylamine+0.44 mL glacial acetic acid,and B was acetonitrile;the detection wavelength:291 nm (0-60 min for phellodendrine),243 nm (60-70 min for astilbin and cyasterone),378 nm (70-80 min for berberine), 336 nm (80-120 min);The column temperature was 30℃ and the sample volume was 10 μL.Eleven modified Sanmiao pills were analyzed by "Similarity Evaluation System for Chromatographic Fingerprint of TCM" (2004 version A).Results: Fingerprint of modified Sanmiao pills was established,and 18 common peaks were identified. Four chemical compounds were identified,including phellodendrine,astilbin,cyasterone,and berberine. Conclusion: The establishment of HPLC fingerprint provided an effective reference for the quality control of modified Sanmiao pills.

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