基于UPLC结合化学计量学方法的龙血竭指纹图谱研究Fingerprint analysis of Resina Draconis from different manufactuers by UPLC coupled with chemometrics
秦建平;李家春;吴建雄;吴素素;黄文哲;王振中;萧伟;
QIN Jian-ping;LI Jia-chun;WU Jian-xiong;WU Su-su;HUANG Wen-zhe;WANG Zhen-zhong;XIAO Wei;Jiangsu Kanion Pharmaceutical Co. ,Ltd.;State Key Laboratory of Pharmaceutical Process New-tech for Chinese Medicine;
摘要(Abstract):
建立不同厂家龙血竭UPLC指纹图谱,为其质量控制提供比较全面的评价方法。采用Phenomenex Kinetex 2.6μC18100A色谱柱,以乙腈-水梯度洗脱,流速1.7 m L·min-1,柱温40℃,检测波长为280 nm。利用化学计量学方法对色谱数据进行相似度分析、聚类分析和主成分分析。采用该方法测定了18批龙血竭,提取15个色谱峰作为指纹图谱共有峰,采用LC-QTOF MS方法指认了13个共有峰;其中15批样品相似度大于0.9;18批样品可大致分为4类。该法重复性好,简便可靠,可以为不同厂家龙血竭的质量控制和评价提供依据。
This study is to establish an UPLC fingerprint of Resina Draconis from different manufacturers,whichcan provide a comprehensive evaluation for its quality control. The analysis was performed on a Phenomenex Kinetex 2. 6 μ C18100 A column by agradientelution program withacetonitrile-water asmobile phase at a flow rate of 1. 7 m L·min-1. The column temperature was 40 ℃ and the detection wavelengthwas 280 nm. The fingerprints of 18 batches of DraconisResina were further evaluated by chemometrics methods including similarity analysis( SA),hierarchical clustering analysis( HCA) and principal component analysis( PCA). As a result,there were 15 common peaks,13 of which had been identified by LC-Q-TOF MS,and the similarity degrees of 15 batches of the samples was more than 0. 9,and the samples were divided into 4 clusters by their quality difference. The method is reproducible,simple and reliablethat it can be used for quality control and evaluation of Resina Draconis from different manufacturers.
关键词(KeyWords):
龙血竭;UPLC;指纹图谱;化学计量学;质量评价
Resina Draconis;UPLC;fingerprint;chemometrics;quality evaluation
基金项目(Foundation): 国家“重大新药创制”科技重大专项(2011ZX09201-201-20)
作者(Author):
秦建平;李家春;吴建雄;吴素素;黄文哲;王振中;萧伟;
QIN Jian-ping;LI Jia-chun;WU Jian-xiong;WU Su-su;HUANG Wen-zhe;WANG Zhen-zhong;XIAO Wei;Jiangsu Kanion Pharmaceutical Co. ,Ltd.;State Key Laboratory of Pharmaceutical Process New-tech for Chinese Medicine;
Email:
DOI:
参考文献(References):
- [1]国家药品监督管理局标准[S].WS3-082(Z-016)-99(Z).
- [2]刘芳,戴荣继,邓玉林,等.龙血竭化学成分研究进展[J].中国药房,2010,21(15):1437.
- [3]高秀丽,蒋倩,王鹏娇,等.龙血竭高效液相色谱特征研究[J].中国中药杂志,2007,32(19):2025.
- [4]周艳林,蒋受军,文建文,等.龙血竭特征成分对照指纹图谱研究[J].中华中医药杂志,2012,27(12):3080.
- [5]颜月园,萧伟,吴云,等.散结镇痛胶囊中黄酮类成分的指纹图谱研究[J].中国实验方剂学杂志,2012,18(5):58.
- [6]胡迎庆,韩慧文,宋月英,等.不同工艺提取龙血竭中紫檀茋的含量测定[J].中成药,2002,24(8):616.
- [7]张晓燕,杨晓明,闫广利,等.龙血竭缓释滴丸的质量标准研究[J].中医药信息,2011,28(2):37.
- [8]李云,萧伟,秦建平,等.HPLC法同时测定龙血竭及其提取物中5个有效成分的含量[J].中国中药杂志,2012,37(7):929.
- [9]王建壮,吕华冲.比色法测定龙血竭总黄酮含量[J].中国实验方剂学杂志,2013,19(16):55.
- [10]秦建平,吴建雄,李家春,等.不同产地龙血竭中5种成分的HPLC法测定[J].现代药物与临床,2013,28(4):265.
- [11]郑庆安.龙血竭研究[D].昆明:中国科学院昆明植物研究所,2003.
- [12]陈慧琴,梅文莉,左文健,等.海南血竭的化学成分研究[J].中国药物化学杂志,2011,21(4):308.
- [13]Yi T,Chen H B,Zhao Z Z,et al.Comparison of the chemical profiles and anti-platelet aggregation effects of two"Draconis Resina"drugs in traditional Chinese medicine[J].J Ethnopharmacol,2011,133:796.
- [14]Baumer U,Dietemann P.Identification and differentiation of Draconis Resina in works of art using gas chromatography/mass spectrometry[J].Anal Bioanal Chen,2010,397:1363.
- [15]Gupta D,Bleakley B,Gupta R K.Draconis Resina:botany,chemistry and therapeutic uses[J].J Ethnopharmacol,2008,115:361.
- [16]Yi T,Tang Y N,Zhang J Y,et al.Characterization and determination of six flavonoids in the ethnomedicine"Draconis Resina"by UPLC-PAD-MS[J].Chem Cent J,2012,6:116.
- 秦建平
- 李家春
- 吴建雄
- 吴素素
- 黄文哲
- 王振中
- 萧伟
QIN Jian-ping- LI Jia-chun
- WU Jian-xiong
- WU Su-su
- HUANG Wen-zhe
- WANG Zhen-zhong
- XIAO Wei
- Jiangsu Kanion Pharmaceutical Co.
- Ltd.
- State Key Laboratory of Pharmaceutical Process New-tech for Chinese Medicine
- 秦建平
- 李家春
- 吴建雄
- 吴素素
- 黄文哲
- 王振中
- 萧伟
QIN Jian-ping- LI Jia-chun
- WU Jian-xiong
- WU Su-su
- HUANG Wen-zhe
- WANG Zhen-zhong
- XIAO Wei
- Jiangsu Kanion Pharmaceutical Co.
- Ltd.
- State Key Laboratory of Pharmaceutical Process New-tech for Chinese Medicine