To determine percentage
13C incorporation two spectra are acquired per sample. One spectrum (
A) contains
1H signals originating from all protons (all
1H spectrum), while the second spectrum (
B) only contains signals from protons attached to a
13C nucleus. The central
13C π–pulse with phase ϕ
3 is executed every second transient in both experiments. The proton magnetisation in the all
1H pulse sequence is the same for
12C and for
13C bound protons and as a consequence, all
1H magnetisation is longitudinal during the interval between
1H pulses with the phases ϕ
2 and ϕ
4. Because of the additional
13C π–pulses in the
13C bound
1H pulse sequence, the magnetisation for the two different kinds of protons develops differently. Here only the
13C bound
1H magnetisation is longitudinal in the interval between the
1H pulses with the phases ϕ
2 and ϕ
4. Therefore, the
12C bound
1H magnetisation can be destroyed using the two pulse field gradients labelled gp
1 and gp
2. A recovery delay of 200 µs was used after each gradient. The central
13C π–pulse with phase ϕ
4 improves magnetisation selection as it is accompanied by phase changes of the
1H pulses and the receiver. All
13C π-pulses are adiabatic Chirp pulses with γB
1max = 10 kHz.
1H,
13C J-coupling is suppressed during acquisition using adiabatic bilevel decoupling (ad-bilev)
21. The pulse phases are: ϕ
1 = x, x, -x, -x; ϕ
2 = x, x, -x, -x for the all
1H spectrum (
A-1) and y, y, y, y for the
13C bound
1H spectrum (
B-1), ϕ
3 = x, y, -x, -y, ϕ
4 = x, -x, -x, x, y, -y, -y, y for the all
1H spectrum (
A-1) and y, -y, -y, y, -x, x, x, -x for the
13C bound
1H spectrum (
B-1). Panels
A-2 and
B-2 show the peaks from Alanine and Lactate methyl protons in the all
1H spectrum (
A-2) and the
13C bound
1H spectrum (
B-2). The scaling of the two spectra is identical allowing easy determination of the percentage incorporation of
13C metabolites. Panels
A-3 and
B-3 demonstrate the complete removal of the
12C bound proton signal from the
13C edited spectrum (B-3) leaving only the natural abundance
13C signals to be observed.