Fig.1

Pulse sequence diagram of 2D JRES NMR experiments

Fig.2

(a) 1H NMR and (b) 2D J-resolved spectra of 200 mmol/L estradiol (dissolved in DMSO-d6) acquired on Varian spectrometer at 500 MHz

Fig.3

PSYCHE based orthogonal-pattern phase-sensitive J-resolved spectroscopy, RASA2DJ. (a) Pulse sequence diagram constituted of 1D PSYCHE and echo-train J acquisition module. A presaturation (Presat) module is adopted before the first nonselective π/2 pulse for water suppression. Vertical bars indicate nonselective π/2 and π pulses, two semicircle shaped pulses with diagonal arrows are frequency-swept chirp pulses with small flip angle β ≪ π/2, G1 and G2 are coherence selection gradients, G3 is a weak gradient matching with chirp pulses, t1 is the indirect evolution period and t2 is the direct acquisition period, SW1 is the spectral width corresponding to t1, and T is the time interval between two adjacent π pulses. (b) The procedure of phase-sensitive processing is illustrated using a singlet peak in a 2D phase-sensitive spectrum, including preserving an original spectrum and generating an F1'-reversed spectrum, summing these two spectra, and performing 1D phase correction along the F2' dimension (Excerpted from Ref. [44])

Fig.4

RASA2DJ experiments on small J coupling systems and complex samples. 1D NMR and RASA2DJ spectra of butyl methacrylate in DMSO-d6 are shown on the left. The total experimental time of RASA2DJ is 4 min. 1D NMR and RASA2DJ spectra of estradiol in DMSO-d6 (part region) are shown on the right. The total experimental time of RASA2DJ is 5 min (Reproduced from Ref. [44])

Fig.5

Pulse sequences for (a) single-band and (b) multi-band OPAM-2DJ experiments. The sequence is constituted of ZS and echo-train J acquisition modules. Green bars denote π/2 and π nonselective pulses, respectively. The red-shaped pulse represents monochromatic π pulse. The yellow-shaped pulses represent polychromatic π/2 and π pulses. Gz indicates the weak gradient for extracting spatial slice-selective signals; G1, G2, G3, G4 are used for coherence pathway selection. Φm, n is the appended Fourier encoding phase. Phase cycling: Φ1 (x, -x), Φ2 (x), Φ3 (x, x, y, y, -x, -x, -y, -y), Φrec (x, y, y, x). Φ4 is varied as (x, x, -x, -x) in the echo-train J acquisition module (Excerpted from Ref. [47])

Fig.6

(a) Conventional 2D JRES and (b) single-band OPAM-2DJ spectra acquired in a inhomogeneous magnetic field (Reproduced from Ref. [47])

Fig.7

High-resolution 2D J-edited spectroscopy applied in inhomogeneous magnetic fields. (a) HR-G-SERF sequence based on 3D acquisition. Phase cycling: Φ1 (x, -x), Φ2 (x), Φ3 (x, x, y, y, -x, -x, -y, -y), Φrec (x, -x, -x, x). (b) AH-G-SERF sequence based on accelerated 2D acquisition from the combination of ZS and G-SERF echo-train acquisition modules. Phase cycling: Φ1=Φ2=Φ3=Φrec=x, and Φ4 is set as a phase array of (x, x, x, x, -x, -x, -x, -x)N/2 in the J-edited echo-train acquisition module. Thin and fat green bars represent π/2 and π nonselective pulses. Blue and red shaped pulses indicate π selective pulses applied for inversing selected proton and spatial frequency encoding, respectively. Gz denotes the weak gradient for spatial frequency encoding. G1, G2, G3, and G4 are coherence-selection gradients (Excerpted from Ref.[53])

Fig.8

High-resolution HR-G-SERF experiments on the complex sample of estradiol under different magnetic field conditions. (a) Molecular conformation and observed coupling networks; (b~d) 1D NMR and HR-G-SERF spectra acquired in a well-shimmed field with selected protons 9 and 15α, respectively; (e~g) 1D NMR and HR-G-SERF spectra acquired in a inhomogeneous with selected protons 9 and 15α, respectively (Reproduced from Ref. [53])