Integrated standardization concept for Angelica botanicals using quantitative NMR.
Integrated standardization concept for Angelica botanicals using quantitative NMR.
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DOI：
10.1016/j.fitote.2011.08.017
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发表时间：
2012-01
期刊：
影响因子：
3.4
通讯作者：
Pauli GF
中科院分区：
文献类型：
--
作者：
Gödecke T;Yao P;Napolitano JG;Nikolić D;Dietz BM;Bolton JL;van Breemen RB;Farnsworth NR;Chen SN;Lankin DC;Pauli GF
尽管有大量的体外/体内和植物化学研究，当归（AS）的活性成分还没有最终确定为标准化的生物活性标志物。在一组体外生物测定中证明活性的AS提取物和级分的植物化学分析一再指出藁本内酯是活性成分（与活性成分相关）。由于藁本内酯的化学不稳定性和GC/LC分析中的相关问题，迫切需要能够定量混合物中藁本内酯的新方法，这些方法不依赖于相同的参比标准品。本研究展示了NMR如何满足同时、多目标定量和定性鉴定的要求。首先，AS活性被浓缩成一个单一的馏分通过RP-固相萃取，证实了（抗）雌激素和细胞毒性试验。接下来，使用标准化合物和比较处理方法建立并验证了定量1H NMR（qHNMR）方法。随后的1D/2D NMR和qHNMR分析导致了活性组分中的藁本内酯和其他次要组分的鉴定和定量，并制定了真实AS制剂的质量标准。通过qHNMR和2D COSY的组合测量了藁本内酯、六种次要烷基苯酞以及苯丙素类、多炔类和多不饱和脂肪酸的绝对和相对量。qNMR方法能够对生物活性组分进行多目标质量控制，并实现AS植物药的综合生物和化学标准化。这种方法可以潜在地转移到具有协同作用的活性成分的其他植物药，或者含有密切相关的和/或成分的其他植物药，这些成分尚未被最终确定为活性成分。
Despite numerous in vitro/vivo and phytochemical studies, the active constituents of Angelica sinensis (AS) have not been conclusively identified for the standardization to bioactive markers. Phytochemical analyses of AS extracts and fractions that demonstrate activity in a panel of in vitro bioassays, have repeatedly pointed to ligustilide as being (associated with) the active principle(s). Due to the chemical instability of ligustilide and related issues in GC/LC analyses, new methods capable of quantifying ligustilide in mixtures that do not rely on an identical reference standard are in high demand. This study demonstrates how NMR can satisfy the requirement for simultaneous, multi-target quantification and qualitative identification. First, the AS activity was concentrated into a single fraction by RP-solid-phase extraction, as confirmed by an (anti-)estrogenicity and cytotoxicity assay. Next, a quantitative 1H NMR (qHNMR) method was established and validated using standard compounds and comparing processing methods. Subsequent 1D/2D NMR and qHNMR analysis led to the identification and quantification of ligustilide and other minor components in the active fraction, and to the development of quality criteria for authentic AS preparations. The absolute and relative quantities of ligustilide, six minor alkyl phthalides, and groups of phenylpropanoids, polyynes, and poly-unsaturated fatty acids were measured by a combination of qHNMR and 2D COSY. The qNMR approach enables multi-target quality control of the bioactive fraction, and enables the integrated biological and chemical standardization of AS botanicals. This methodology can potentially be transferred to other botanicals with active principles that act synergistically, or that contain closely related and/or constituents, which have not been conclusively identified as the active principles.
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影响因子：
5.8
作者：
Cheah, Yew Hoong;Nordin, Fariza Juliana;Sarip, Rozie;Tee, Thiam Tsui;Azimahtol, Hawariah Lope Pihie;Sirat, Hasnah M.;Abd Rashid, Badrul Amini;Abdullah, Noor Rain;Ismail, Zakiah
通讯作者：
Ismail, Zakiah
影响因子：
5.1
作者：
Pauli, Guido F.;Jaki, Birgit U.;Lankin, David C.
通讯作者：
Lankin, David C.
影响因子：
1.7
作者：
Choi, YH;Choi, HK;Verpoorte, R
通讯作者：
Verpoorte, R
DOI：
10.1002/mrc.2526
发表时间：
2009-12
期刊：
Magnetic resonance in chemistry : MRC
影响因子：
--
作者：
Lewis IA;Schommer SC;Markley JL
通讯作者：
Markley JL
影响因子：
3.3
作者：
Deng, Shixin;Chen, Shao-Nong;Pauli, Guido F.
通讯作者：
Pauli, Guido F.