Table 3.

Application of analytical approaches in longitudinal nutritional studies.

Bioactive Compound, Extract or Supplement	Analytical Technique	Biological Samples	Population	Dose/Intervention	Results	Ref
Catechin	LC(RP)-QTOF–MS	Plasma, urine, heart, liver and aorta	24 male Wistar rats divided in different groups	Diet supplemented or not with 0.2% (+)-catechin.	76 variables affected by catechin supplementation	[125]
Resveratrol	UPLC(RP)-Orbitrap–MS/MS GC-EI-Q–MS	Blood, urine, adipose tissue, skeletal muscle tissue	66 men subjects with metabolic syndrome	(a)75 mg twice daily (b)500 mg twice daily (c)Placebo Duration: 4 months	Reduced sulphated androgen precursors, long-chain PUFAs (n-3 and n-6) increased in adipose tissue,	[126]
Vitamin E	LC(RP)–MS(QTOF)	Plasma samples	10 male adults	400 mg/d of RRR-α-tocopheryl acetate (4 weeks)	Influence in phospholipid metabolism and lysoPC generation	[124]
Cocoa (Theobroma cacao L.)	LC(RP)-QQQ–MS/MS	24 h urine and fasting plasma samples	19 men and 23 women presenting high risk of cardiovascular heart disease	(a)20 g/day of cocoa powder with 250 mL skimmed milk (b)Placebo (500 mL/day of skimmed milk) Duration: 4 weeks	Increase in the urinary excretion of colonic microbial-derived phenolic metabolites, and biomarkers of the intake.	[135]
Chamomile extract	1H NMR	Urine samples	14 healthy volunteers	5 g of powder in 200 mL of boiling water (5 times/day). Duration: 2 weeks	Depletion of creatinine and the elevation of hippurate, glycine	[142]
Curcuma longa extract (1% of curcuminoids)	1H NMR, GC-ITQ–MS (Fatty acids)	Serum samples	30 rats (animal model)	(a)HFS diet with a Curcuma longa extract. (b)HFS diet (control) (c)standard diet Duration: 10 weeks	Metabolic differences in MUFA, n-3 PUFA, glycoproteins, glutamine and methanol (fatty acid metabolism)	[127]
Rosemary extract	LC(RP)-QTOF–MS	Urine samples	30 streptozotocin-induced diabetic rats	R.officinalis (150 mg) plus folic acid (15 mg)	Several amino acids and their metabolites point to changes due to the effect of the gut microbiota	[128]
Soy	GC-Q–MS	Fecal samples	35 female rats	SOY diet (590 mg/kg od soy isoflavones) or placebo. Duration: 29 weeks	SOY-fed animals had greater fecal concentrations of the beneficial bacterial metabolite, S-equol	[143]
Soy beef and grapefruit juice	1H NMR	Serum samples	25 healthy male volunteers	140 g of soy bean beefs and 500 mL of grapefruit juice per day for four consecutive days	Decrease of lactate, cholesterols and triglycerides	[131]
Probiotic fermented milk	1H NMR	Serum and fecal samples	74 patients with irritable bowel syndrome	Probiotic fermented milk (150 mL) or placebo 3/times daily for 8 weeks	Dysregulation in energy homeostasis (serum glucose) and liver function (serum tyrosine)	[134]
Supplement based on polyphenols from wine and red grape	GC-TOF–MS	Blood, 24 h urine, and fecal samples	26 adult human volunteers	Cellulose capsules with a polyphenol-rich mix of red wine and red grape juice extracts (800 mg of polyphenols) or placebo. Duration: 4 weeks	Increase of phenolic acids and evaluation of the gut microbial impact	[132]
Functional food based on grape skin polyphenols	LC(RP)-QTOF–MS	24 h urine samples	31 volunteers	187 mL of the functional beverage, containing a grape skin extract Control beverage as a placebo Duration: 15 days	Presence offirst-stage microbial metabolites of flavanols Several epicatechin and phenolic acid metabolites as markers of the intake	[116]
Red wine and grape juice extracts (WGM)	GC-Q–MS LC(RP)-QQQ–MS	Urine and plasma samples	35 healthy males	WGM in gelatin capusles (870 mg of dry weight red wine extract and 540 mg of dry weight grape juice extract) or placebo. Duration: 5 days	Alteration of microbial protein fermentation and amino acid metabolism (tyrosine, tryptophan).	[129]
Garlic (allium sativum) supplement Aliocare®	LC(RP)-ESI-QTOF–MS	Plasma samples	30 healthy volunteers (15 men and 15 women)	One gelatine capsule contained per day (70 mg of garlic supplement). Duration: 1 month	Increase in lysophosphatidylcholines, lysophosphatidylethanolamines and acylcarnitines. Decrease of four fructosamines	[130]