Capillary HPLC-NMR coupling high-resolution NMR spectroscopy in the nanoliter scale

被引:76
作者
Behnke, B
Schlotterbeck, G
Tallarek, U
Strohschein, S
Tseng, LH
Keller, T
Albert, K
Bayer, E
机构
[1] UNIV TUBINGEN,INST ORGAN CHEM,D-72076 TUBINGEN,GERMANY
[2] BRUKER ANALYT MESSTECH GMBH,D-76287 RHEINSTETTEN,GERMANY
关键词
D O I
10.1021/ac950925a
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
Coupling HPLC and NMR is one of the most powerful techniques for simultaneous separation and structural elucidation of unknown compounds in mixtures, To date, however, minimizing the detection volume, as is required when coupling NMR with miniaturized separation techniques, has been accompanied by a dramatic loss in resolution of the NMR spectra, Here, we report on the coupling of gradient capillary HPLC with on-column, high-resolution NMR detection. On-line stopped-flow and static H-1 NMR spectra were acquired with capillary columns of 75-315 mu m i.d. With detection over a length of 1.2 cm, cell volumes cover a range of 50-900 nL, An on-line-detected NMR separation of dansylated amino acids was carried out in a 315 mu m i.d. fused silica capillary packed to a length of 12 cm with C-18 stationary phase, The low solvent consumption makes the use of fully deuterated solvents economically feasible. NMR spectra with resolution on the order of 3 Hz were obtained using a 50 nL detection cell to measure 1.1 nmol of dansylated gamma-aminobutyric acid under static conditions in a 75 mu m i.d. capillary.
引用
收藏
页码:1110 / 1115
页数:6
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