HPLC-NMR revisited: Using time-slice HPLC-SPE-NMR with database assisted dereplication
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HPLC-NMR revisited: Using time-slice HPLC-SPE-NMR with database assisted dereplication. / Johansen, Kenneth; Wubshet, Sileshi Gizachew; Nyberg, Nils.
In: Analytical Chemistry, Vol. 85, No. 6, 2013, p. 3183-3189.Research output: Contribution to journal › Journal article › Research › peer-review
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TY - JOUR
T1 - HPLC-NMR revisited: Using time-slice HPLC-SPE-NMR with database assisted dereplication
AU - Johansen, Kenneth
AU - Wubshet, Sileshi Gizachew
AU - Nyberg, Nils
PY - 2013
Y1 - 2013
N2 - Time based trapping of chromatographically separated compounds on to solid-phase extraction cartridges (SPE) and subsequent elution to NMR-tubes was done to emulate the function of HPLC–NMR for dereplication purposes. Sufficient mass sensitivity was obtained by the use of a state-of-the-art HPLC–SPE–NMR-system with a cryogenically cooled probe head, designed for 1.7 mm NMR-tubes. The resulting 1H NMR spectra (600 MHz) were evaluated against a database of previously acquired and prepared spectra. The in-house developed matching algorithm, based on partitioning of the spectra and allowing for changes in the chemical shifts, is described and the code included as Supplementary Information. Two mixtures of natural products was used to test the approach; one extract of Carthamus oxyacantha (wild safflower) containing an array of spiro compounds and one extract of the endophytic fungus Penicillum namyslowski containing griseofulvin and analogues. The database matching of the resulting spectra positively identified expected compounds, while the number of false positives was few and easily recognized.
AB - Time based trapping of chromatographically separated compounds on to solid-phase extraction cartridges (SPE) and subsequent elution to NMR-tubes was done to emulate the function of HPLC–NMR for dereplication purposes. Sufficient mass sensitivity was obtained by the use of a state-of-the-art HPLC–SPE–NMR-system with a cryogenically cooled probe head, designed for 1.7 mm NMR-tubes. The resulting 1H NMR spectra (600 MHz) were evaluated against a database of previously acquired and prepared spectra. The in-house developed matching algorithm, based on partitioning of the spectra and allowing for changes in the chemical shifts, is described and the code included as Supplementary Information. Two mixtures of natural products was used to test the approach; one extract of Carthamus oxyacantha (wild safflower) containing an array of spiro compounds and one extract of the endophytic fungus Penicillum namyslowski containing griseofulvin and analogues. The database matching of the resulting spectra positively identified expected compounds, while the number of false positives was few and easily recognized.
U2 - 10.1021/ac303455j
DO - 10.1021/ac303455j
M3 - Journal article
C2 - 23432092
VL - 85
SP - 3183
EP - 3189
JO - Industrial And Engineering Chemistry Analytical Edition
JF - Industrial And Engineering Chemistry Analytical Edition
SN - 0003-2700
IS - 6
ER -
ID: 44521856