摘要
目的:建立指纹图谱,并采用一测多评法测定正天丸中升麻素苷、5-O-甲基维斯阿米醇苷、阿魏酸、欧前胡素、异欧前胡素5个化学成分含量。方法:采用高效液相色谱法测定12批正天丸的指纹图谱,建立指纹图谱共有模式。以欧前胡素为内参物,建立升麻素苷、5-O-甲基维斯阿米醇苷、阿魏酸和异欧前胡素的相对校正因子,并进行含量计算,实现一测多评;同时采用外标法测定12批正天丸中5种化学成分的含量,比较计算值与实测值的差异,验证一测多评法的准确性。色谱条件:采用Dimonsil C_(18)(2)色谱柱(4.6 mm×250 mm,5μm),以乙腈(A)-0.095%磷酸水溶液(B)为流动相,梯度洗脱(0~5 min,10%A→20%A;5~40 min,20%A→40%A;40~50 min,40%A;50~65 min,40%A→70%A;65~70 min,70%A),流速1.0 mL·min^(-1),检测波长310 nm,柱温30℃。结果:12批正天丸指纹图谱标定了共有峰34个,指认了其中5个化学成分。12批样品指纹图谱与对照指纹图谱的相似度均大于0.990。建立的相对校正因子重现性良好,采用校正因子计算的含量值与实测值之间无显著性差异(P>0.05)。结论:所建立的方法可用于正天丸中升麻素苷、5-O-甲基维斯阿米醇苷、阿魏酸、欧前胡素、异欧前胡素5个化学成分的定性定量分析。
Objective:To establish fingerprint of Zhengtian pills and to develop quantitation method of five lignanoids(prim-O-glucosylcimifugin,5-O-methylvisammioside,ferulic acid,imperatorin and isoimperatorin) by single-marker.Methods:12 batches of Zhengtian pills were determined by HPLC and a common fingerprint was established.Quantitative analysis of multi-components by single-marker(QAMS) was performed.Imperatorinwas selected as internal reference and the relative correction factors(RCF) of other four components to it were calculated.The QAMS method was evaluated by external standard method.The analysis was carried out on an analytical column of Dimonsil C18(2)(4.6 mm×250 mm,5 μm) with gradient elution by acetonitrile(A)-0.095% phosphoric acid solution(B)(0-5 min,10%A → 20%A;5-40 min,20%A → 40%A;40-50 min,40%A;50-65 min,40%A → 70%A;65-70 min,70%A),at a flow rate of 1.0 mL·min^-1.The detection wavelength was 310 nm and the column temperature was 30 ℃.Results:There were 34 common peaks in fingerprints of 12 batches of Zhengtian pills,five of which were identified.The similarities of fingerprints were over 0.990.The established RCF had a good reproducibility.No significant differences(P〉0.05) were found between the quantitative results of external standard method and QAMS method.Conclusion:The developed method can be used for the qualitative and quantitative analysis of prim-O-glucosylcimifugin,5-O-methylvisammioside,ferulic acid,imperatorin and isoimperatorin in Zhengtian pills.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第1期79-88,共10页
Chinese Journal of Pharmaceutical Analysis
关键词
正天丸
指纹图谱
一测多评法
升麻素苷
甲基维斯阿米醇苷
阿魏酸
欧前胡素
异欧前胡素
Zhengtian pills
fingerprint
quantitative analysis of multi'components by single.marker ( QAMS )
prim-O-glucosylcimifugin
methylvisammioside
ferulic acid
imperatonn
isoimperatorin