Patent ID: 6498040
Filing Date: 2002-12-24
Classification: G01N,G01R,Y10T

Abstract:
A process for mobile phase conversion in high-performance liquid chromatography (HPLC) to carry out separation and preparation of a sample for NMR analysis, comprising the steps of:separating a target ingredient from other ingredients contained in the sample by a high-performance liquid chromatography process with a separation column and a first mobile phase; trapping said target ingredient in a trapping column using a second mobile phase that is different from said first mobile phase; replacing said second mobile phase in said trapping column with deuterium oxide; and eluting said target ingredient from said trapping column using a deuterated solvent other than said deuterium oxide, said separating step further comprising a step of actuating a pump (P1) to supply said first mobile phase for separation of the sample in said separation column, a detector to detect a peak of said target ingredient, and valves (V1), (V2), (V3), wherein said target ingredient flows through said valve (V1) into a sampling loop (LOOP) extending between said valve (V2) and said valve (V3) so as to be accumulated in said sampling loop (LOOP); said trapping step further comprising a step of actuating a pump (P2) to supply said second mobile phase for concentration of the sample so as to flow through said valve (V1), said valve (V2), said sampling loop (LOOP), said valve (V3), a valve (V4), a valve (V5), said trapping column (TC) and said valve (V4) in this order, and a distribution valve (R) serving to mix the target ingredient accumulated in said sampling loop with said second mobile phase for concentration of the sample between said valve (V3) and said valve (V4) so that the target ingredient may be concentrated in said trapping column (TC); said replacing step further comprising a step of actuating a pump (P3) to supply deuterium oxide so as to flow through said valve (V5), said trapping column (TC) and said valve (V4) in this order and to replace said second mobile phase with deuterium oxide; and said eluting step further comprising a step of actuating a pump (P4) to supply deuterated solvent other than deuterium oxide so as to flow through said valve (V4), said trapping column (TC), said valve (V5), said valve (V4), said separation column (AC) and a detector (D2) so that the target ingredient may be obtained for NMR analysis.