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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nifdc.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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HPLC-ESI/MS法测定续断"发汗"前后绿原酸和川续断皂苷Ⅵ的含量

Determination of chlorogenic acid and asperosaponin Ⅵ in crude and sweated Radix Dipsaci by HPLC-ESI/MS

分类号:
出版年·卷·期(页码):2013,33 (1):0-0
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的: 建立续断"发汗"前后绿原酸和川续断皂苷Ⅵ的高效液相色谱-电喷雾-三重四极杆质谱联用测定方法。方法: 采用Agilent Zorbax SB C18(3.5 mm×100 mm,3.5 μm)色谱柱,以水(A)-甲醇(B)为流动相,梯度洗脱(0~3 min,60%B→100%B;3~7 min,100%B;7~10 min,100%B→60%B)。绿原酸以m/z 353.0为母离子,m/z 191.0、127.0为子离子,川续断皂苷Ⅵ以m/z 927.5为母离子,m/z 603.3、323.3为子离子,采用多反应监测(MRM)负离子模式对续断"发汗"前后进行检测。结果: 5个不同批次的续断经"发汗"后,绿原酸含量均有所降低,分别降低了41.18%、20.54%、20.51%、54.27%、5.02%;川续断皂苷Ⅵ的含量均有所增加,分别增加了15.45%、1.18%、12.08%、9.22%、119.72%。结论: 产地加工—"发汗"影响续断中绿原酸和川续断皂苷Ⅵ的含量,实验结果为进一步研究"发汗"机理提供依据。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To establish an HPLC-electrospray ionisation tandem QQQ mass spectrometry method for simultaneous determination of chlorogenic acid and asperosaponin Ⅵ in crude and sweated Radix Dipsaci. Methods: The two components were analyzed simultaneously with a Zorbax C18 column by gradient elution using water-methanol as the mobile phase (0-3 min, 60%B→100%B;3-7 min, 100%B;7-10 min, 100%B→60%B).The mass spectrometer was operated in the negative-ion mode using multiple reaction monitoring (MRM), and the precursor ion of chlorogenic acid at m/z 353.0 yielded two main daughter ions of m/z 191.0, 127.0, and the precursor ion of asperosaponin Ⅵ at m/z 927.5 yielded two main daughter ions of m/z 603.3, 323.3. Results: After being sweated, the content of chlorogenic acid in five batches of Radix Dipsaci decreased by 41.18%, 20.54%, 20.51%, 54.27%, 5.02%, respectively, and the content of asperosaponin Ⅵ increased by 15.45%, 1.18%, 12.08%, 9.22%, 119.72%, respectively. Conclusion: The method of origin processing "sweating" could change the contents of chlorogenic acid and asperosaponin Ⅵ in Radix Dipsaci.The experimental results provided the basis for further study on sweating mechanism.

-----参考文献:---------------------------------------------------------------------------------------
1 ChP(中国药典).2010.Vol Ⅰ(一部):309
2 YANG Zhong-lin(杨中林),LIU Shuang-yue(刘双跃),QIN Min-jian(秦民坚).Influence of different processing methods on the changes of Akebia Saponin D in Radix Dipsaci(不同加工方法对续断中Akebia Saponin D含量变化的影响).Inf Tradit Chin Med(中医药信息),2000(1):16
3 WANG Xia(汪霞).Comparative study on the no-sweated and sweated Radix Dipsaci(发汗与不发汗续断的比较研究).Zhejiang J Chin Tradit Med(浙江中医杂志),2011,46(4):292
4 WANG Chu(王初).Comparison on the contens of water-soluble extractives and asperosaponin Ⅵ in no-sweated and sweated Radix Dipsaci(发汗与不发汗续断中水溶性浸出物和川续断皂苷Ⅵ的比较).Chin Tradit Herb Drugs(中草药),2007,38(6):865
5 TAN Hong-gen(谭洪根),LIN Sheng(林生),ZHANG Qi-wei(张启伟),et al.Determination of akebiasaponin D in root of Dipacus asperoides by HPLC(高效液相色谱法测定续断药材中川续断皂苷Ⅵ的含量).China J Chin Mater Med(中国中药杂志),2006,31(9):726
6 MA Xin-fei(马新飞),LU Tu-lin(陆兔林),MAO Chun-qin(毛春芹),et al.Determination of asperosaponin Ⅵ in different processed products of Radix Dipsaci by HPLC(HPLC法测定不同续断炮制品中川续断皂苷Ⅵ).Chin Tradit Herb Drugs(中草药),2007,38(5):707
7 DONG Wen-san(董文桑),QU Fa-lin(瞿发林),JIANG Yan(蒋燕).Determination of asperosaponin Ⅵ in Shujing Huoluo spirit by HPLC(HPLC法测定舒筋活络酒中川续断皂苷Ⅵ含量).China Pharm(中国药师),2008,11(3):284
8 XIA Li-wu(夏立武),TANG Xiao-xia(唐晓霞),LIU Ya-jun(刘亚军),et al.HPLC determination of asperosaponin Ⅵ in Shushen Yiqi Zhixue granules(HPLC测定熟参益气止血颗粒中川续断皂苷Ⅵ的含量).Chin J Pharm Anal(药物分析杂志),2011,31(5):941
9 JIN Qi(金奇),LAI Ping-fan(来平凡),DU Wei-feng(杜伟锋),et al.Effects of primary processing on quality of Dipsacus asperoides("发汗"对续断质量的影响).Chin Arch Tradit Chin Med(中华中医药学刊),2012,29(12):2636

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