HPLC-DAD-ESI-MS/MS研究金银花水提工艺中绿原酸类成分的变化规律Regularity of changes in chlorogenic acids in Lonicera japonica extracts by HPLC-DAD-ESI-MS/MS
张倩;张加余;隋丞琳;史新元;乔延江;卢建秋;
ZHANG Qian1,2,ZHAGN Jia-yu2,SUI Cheng-lin2,SHI Xin-yuan2,QIAO Yan-jiang2,LU Jian-qiu1(1.Center of Scientific Experiment,Beijing University of Chinese Medicine,Beijing 100029,China; 2.School of Chinese Pharmacy,Beijing University of Chinese Medicine,Beijing 100102,China)
摘要(Abstract):
目的:分析金银花水提液中的绿原酸类成分及水提过程中绿原酸类成分的变化规律。方法:Agilent Zorbax SB-C18色谱柱(4.6 mm×250 mm,5μm),检测波长327 nm,柱温30℃,流动相0.1%甲酸溶液(A)-乙腈(B),梯度洗脱,流速0.5mL.min-1,质谱采用负离子多级检测模式,对抽取的22个金银花水提液样本进行分析。结果:从水提液中准确鉴定了咖啡酸和6种绿原酸类成分。在提取过程中,绿原酸和3,5-二咖啡酰奎宁酸含量达到最高值后会逐渐趋于平衡或缓慢降低,其他成分的含量一直呈上升趋势,但是变化率逐渐减小。结论:该研究为改进含金银花中药制剂的生产工艺提供了依据。
Objective: To analyze chlorogenic acids contained in Lonicera japonica water extracts,and to investigate the regularity of changes in chlorogenic acids during the water extraction process.Method: Agilent Zorbax SB-C18 analytical column(4.6 mm×250 mm,5 μm) was eluted with 0.1% formic acid(A)-acetonitrile(B) as the mobile phase at a flow rate of 0.5 mL·min-1.The detection wavelength was 327 nm and the column temperature was 30 ℃.Negative MSn mode was adopted in mass spectrum for ananlyzing the 22 samples of L.japonica water extracts.Result: Caffeic acid and six organic acids were accurately identified from the water extracts.During the extraction,the contents of chlorogenic acid and 3,5-dicaffeoylquinic acid became stable or gradually decreased after reaching the highest value.The contents of other components had long been increasing,but with a decreasing rate of change.Conclusion: This study provides basis for improving the production process of traditional Chinese medicine preparations containing L.japonica.
关键词(KeyWords):
金银花;水提工艺;绿原酸类成分;HPLC-DAD-ESI-MS/MS;变化规律
Lonicera japonica;water extraction process;chlorogenic acids;HPLC-DAD-ESI-MS/MS;regularity of change
基金项目(Foundation): 国家“重大新药创制”科技重大专项(2010ZX09502-002);; 北京中医药大学自主选题项目(2011-JYBZZ-XS104)
作者(Authors):
张倩;张加余;隋丞琳;史新元;乔延江;卢建秋;
ZHANG Qian1,2,ZHAGN Jia-yu2,SUI Cheng-lin2,SHI Xin-yuan2,QIAO Yan-jiang2,LU Jian-qiu1(1.Center of Scientific Experiment,Beijing University of Chinese Medicine,Beijing 100029,China; 2.School of Chinese Pharmacy,Beijing University of Chinese Medicine,Beijing 100102,China)
参考文献(References):
- [1]王燕,王智民,林丽美,等.金银花及其同属植物化学成分研究进展[J].中国中药杂志,2008,33(8):968.
- [2]陈有根,王志斌,戴俊东.3种经典工艺生产的金银花提取物中绿原酸类成分含量比较[J].中成药,2007,29(3):362.
- [3]刘意,曾桂先,宋凤兰,等.绿原酸稳定性研究[J].辽宁化工,2009,38(4):226.
- [4]李小芩,孙晓红,蔡爽,等.采用UPLC-ESI-MS/MS以及主成分聚类分析研究不同品种金银花的化学成分及其差异[J].药学学报,2009,44(8):895.
- [5]田晨煦,徐小平,廖丽云,等.高效液相色谱-串联质谱法分离鉴定绿原酸及其相关杂质[J].色谱,2007,25(4):496.
- [6]张丽媛,李遇伯,李利新,等.RRLC-Q-TOF/MS分析金银花的化学成分[J].中南药学,2012,10(3):204.
- [7]阎东海.提取三要素在金银花提取过程中对氯原酸提出率及稳定性的相关性研究[J].中国中药杂志,1994,19(9):545.
- [8]刘永刚,卢建秋,高晓燕,等.高效液相色谱-电喷雾电离质谱法分析不同时期金银花中酸性成分及含量[J].中国药房,2006,17(22):1756.
- [9]罗奇志,王有至,罗佳波.绿原酸水解产物的高效液相色谱-电喷雾串联质谱分析[J].药物分析杂志,2011,31(7):1345.
- [10]Ma Yuan-chun,Wang Xiao-qian,Hou Fei-fei,et al.Rapid res-olution liquid chromatography(RRLC)analysis and studies onthe stability of Shuang-Huang-Lian preparations[J].J Pharm Bi-omed Anal,2011,54:265.
- [11]陈俊.金银花提取物的物质基础和制备工艺研究[D].杭州:浙江大学,2010.
- 金银花
- 水提工艺
- 绿原酸类成分
- HPLC-DAD-ESI-MS/MS
- 变化规律
Lonicera japonica - water extraction process
- chlorogenic acids
- HPLC-DAD-ESI-MS/MS
- regularity of change
- 张倩
- 张加余
- 隋丞琳
- 史新元
- 乔延江
- 卢建秋
ZHANG Qian1- 2
- ZHAGN Jia-yu2
- SUI Cheng-lin2
- SHI Xin-yuan2
- QIAO Yan-jiang2
- LU Jian-qiu1(1.Center of Scientific Experiment
- Beijing University of Chinese Medicine
- Beijing 100029
- China
- 2.School of Chinese Pharmacy
- Beijing University of Chinese Medicine
- Beijing 100102
- China)
- 张倩
- 张加余
- 隋丞琳
- 史新元
- 乔延江
- 卢建秋
ZHANG Qian1- 2
- ZHAGN Jia-yu2
- SUI Cheng-lin2
- SHI Xin-yuan2
- QIAO Yan-jiang2
- LU Jian-qiu1(1.Center of Scientific Experiment
- Beijing University of Chinese Medicine
- Beijing 100029
- China
- 2.School of Chinese Pharmacy
- Beijing University of Chinese Medicine
- Beijing 100102
- China)