Table 1.

Assignments of resonances in the 600 MHz ¹H NMR spectra of WMS supernatant samples for the expanded δ = 0.80–2.45 and 5.10–8.60 ppm regions only. Chemical shift (ö) values and resonance coupling patterns are also provided. * Indicates tentative assignment. Resonances and their assignments within the 2.45–5.10 ppm regions of spectra (signals 47–95) are omitted for the purpose of clarity, but these may be viewed in Part I of this series of reports [1].

Assignment Code	Chemical Shift (δ/ppm)	Coupling Pattern	Assignment
1	0.861	t	n-Caproate-CH3
2	0.885	d	iso-Valerate-CH3′s
3	0.893	t	n-Butyrate-CH3
7	0.962	t	Leucine-CH3
8	0.982/0.996	2 × d	Valine-CH3/Isoleucine-CH3
10	1.035	d	Valine-CH3
11	1.058	t	Propioniate-CH3
12	1.125	d	iso-Butyrate-CH3
13	1.150	d	3-Amino-iso-butyrate-CH3
15	1.183	t	Ethanol-CH3
16	1.211	d	Methylmalonate-CH3/α-Fucose
17	1.242	d	3-D-hydroxybutyrate-CH3/β-Fucose
18	1.330	d	Lactate-CH3
19	1.371	d	Acetoin-CH3
20	1.486	d	Alanine-CH3
21	1.551	q	n-Butyrate-β-CH2
22	1.641	m	5-Aminovalerate-β,γ-CH2′s
Lys	1.71	m	Lysine-δ-CH2
25	1.76	m	Putrescine-β-CH2
26	1.77	m	Ornithine-β-CH2/Propane-1,3-diol-CH2-β-CH2
Asat	1.813/2.026	2 × s	Acetate-CH3 13C satellite signals
β-NAcN-C3Hax	1.83	pseudo-dd	β-N-Acetylneuraminate-C3H position axial proton
30	1.92	s	Acetate-CH3
31	1.954	m	* 2-Hydroxyglutarate-γ-CH2
32	2.005	m	Proline-γ-CH2/N-Acetylneuraminate-C3H
33	2.02–2.080	broad	Glycoprotein-/Hyaluronate-/Glycoprotein carbohydrate side-chain N-acetylsugar-NHCOCH3 functions
34	2.025/2.030	s	N-Acetylglutamate-/N-Acetylaspartate-NHCOCH3 (2 signals)
β-Nac-CH3	2.041	s	β-N-Acetylglucosamine-NHCOCH3
β-NacN	2.06	s	β-N-Acetylneuraminate-NHCOCH3
37	2.098	s	Dimethylsulphide-S-CH3
38	2.140	s	Methionone-S-CH3
39	2.164	t	n-Butyrate-α-CH2
40	2.193	q	Propioniate-CH2
41	2.215	s	Acetone-CO-CH3
42	2.235	t	5-Aminovalerate-α-CH2
AcAc	2.27	s	Acetocaetate-CH3
2-OG	2.331	t	2-Oxoglutarate-4-CH2
43	2.334	m	Glutamate-γ-CH2
44	2.377	s	Pyruvate-CH3
Ox	2389	s	Oxaloacetate-CH2
46	2.415	s	Succinate-CH2
α-Fuc	5.209	d	α-Fucose-C1H
α-Glc	5.232	d	α-Glucose-C1H
UPH	5.24	m	Unassigned polyhroxy- species
96	5.392	s	Allantoin-CH
Sucr	5.414	d	Sucrose-C1H
CD-CH=CH	5.62	m	Conjugated diene species olefinic proton
97	5.67	s	Unassigned
98	5.79	broad (s)	Urea-CO-NH2
99	5.800	d	Uracil-C2H
Cinn	6.375	d	Cinnamate derivative-CH=CH-Ar
100	6.52	s	Fumarate-CH=CH-
101	6.84	d	4-Hydroxyphenylacaetate aromatic ring-C3H/C5H
102	6.85	broad	* Protein aromatic amino acid residue(s)
103	6.880	d	Tyrosine aromatic ring-C2H/C6H
104	7.071	s	Histidine imidazole ring-C5H
104A	7.155	d	4-hydroxyphenylacetate aromatic ring-C2H/C6H
105	7.237	d	Tyrosine aromatic ring-C3H/C5H
106	7.320	m	Phenylalanine aromatic Ring-C2H/C6H
107	7.375	m	Phenylalanine aromatic ring-C4H
108	7.43	m	Phenylalanine aromatic ring-C3H/C5H
109	7.533	d	Uracil-C1H
110	7.552	m	* Protein aromatic amino acid residue(s)
111	7.812	s	Histidine imidazole ring-C2H
112	7.913	s	3-Methylhisitidine imidazole ring-C2H
113	8.05	2 × broad signals	* Protein aromatic amino acid residue(s)
114	8.175	s	Hypoxanthine-C8H
115	8.219	s	Hypoxanthine-C3H
116	8.456	s	Formate-CH