摘要
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-C_(18)(4.6 mm×250 mm,5μm)色谱柱,以0.1%三乙胺水1 000 m L+冰醋酸0.44 m L为流动相A,乙腈为流动相B,梯度洗脱,流速1 m L·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10μL。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 × 250mm, 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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2016年第8期1377-1384,共8页
Chinese Journal of Pharmaceutical Analysis
基金
国家自然科学基金面上项目(81374048)
浙江省中医药科技计划项目(2015ZA062)
国家级大学生创新创业训练计划项目(2016-751610V002)
关键词
加味三妙丸
中药复方指纹图谱
黄柏碱
落新妇苷
杯苋甾酮
小檗碱
黄柏
苍术
川牛膝
土茯苓
高效液相色谱
modified Sanmiao pills
fingerprint of Chinese herbal formula
phellodendrine
astilbin
eyasterone
berberine
Cortex Phellodendri
Rhizoma Atractylodis
Radix Cyathulae
Rhizoma Smilacis Glabrae
HPLC
