Identification of Natural Products Using HPLC-SPE Combined with CapNMR
详细信息 查看全文
- 作者：Maja Lambert ; Jean-Luc Wolfender ; Dan Stæ ; rk ; S. Br<img src="http ; //pubs.acs.org/images/gifchars/oslash.gif" border="0">gger Christensen ; Kurt Hostettmann ; Jerzy W. Jaroszewski
- 刊名：Analytical Chemistry
- 出版年：2007
- 出版时间：January 15, 2007
- 年：2007
- 卷：79
- 期：2
- 页码：727 - 735
- 全文大小：548K
- 年卷期：v.79,no.2(January 15, 2007)
- ISSN：1520-6882
文摘
Two major development areas in HPLC-NMR hyphenationare postcolumn solid-phase extraction (HPLC-SPE-NMR)and capillary separations with NMR detection by meansof solenoidal microcoils (CapNMR). These two techniqueswere combined off-line into HPLC-SPE-CapNMR, whichcombines the advantage of high loadability of normal-boreHPLC columns with high mass sensitivity of capillaryNMR probes with an active volume of 1.5 <IMG SRC="/images/entities/mgr.gif">L. Thetechnique was used for rapid identification of complexsesquiterpene lactones and esterified phenylpropanoidspresent in an essentially crude plant extract (toluenefraction of an ethanolic extract of Thapsia garganicafruits). Elution profiles of 10 × 1 mm i.d. SPE cartridgesfilled with poly(divinylbenzene) resin were found to beonly marginally broader than those observed upon directinjection of 6-
L samples into the probe. Thus, thetechnique focuses analytes emerging in the HPLC elutionbands of 0.5-1 mL into volumes of ~10 L, compatiblewith the CapNMR probe. Using this technique, ninenatural products (1-9) present in the plant extract inamounts varying from 0.1 to 20% were identified bymeans of 1D and 2D NMR spectra, supported by parallelHPLC-ESIMS measurements. Therefore, HPLC-SPE-CapNMR should be regarded as an attractive alternative toother applications of CapNMR for mixture analysis.
L samples into the probe. Thus, thetechnique focuses analytes emerging in the HPLC elutionbands of 0.5-1 mL into volumes of ~10 L, compatiblewith the CapNMR probe. Using this technique, ninenatural products (1-9) present in the plant extract inamounts varying from 0.1 to 20% were identified bymeans of 1D and 2D NMR spectra, supported by parallelHPLC-ESIMS measurements. Therefore, HPLC-SPE-CapNMR should be regarded as an attractive alternative toother applications of CapNMR for mixture analysis.