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Table 1 List of studies reporting candidate biomarkers for grape/raisin and berry consumption

From: Food intake biomarkers for berries and grapes

Dietary factor

Study design

Number of subjects

Analytical method

Sample type

Discriminating metabolites/candidate biomarkers

Reference(s)

Grapes and raisins

  Red grapes (50–200 g)

Single-dose study, short-term controlled study (4 days), crossover design

6 (3 F, 3 M)

NMR

Urine (0–24 h after intake)

• Tartaric acid

[66]

19 (9 F, 10 M)

NMR

Urine (fasting & 24–h urine)

  Grape juice (200–1200 mL)

Single dose study

1 M

LC-MS

Urine (0–4 h after intake)

• Resveratrol

[107]

  Grape juice (12–18 oz)

Intervention study

2 M

NMR

Urine (overnight)

• Tartaric acid

[96]

  Grape juice (28 mL)

Intervention study

23 (not specified)

LC-MS

Urine (overnight)

• Tartaric acid

[97]

  Red grape juice (1 L)

Single-dose study, crossover design

11 M

GC-MS

Plasma (0–24 h after intake)

Urine (0–24 h after intake)

• cis-Resveratrol

• trans-Resveratrol

[121]

  Red grape juice (Concord) (350 mL)

Single-dose study

12 (7 F, 5 M)

GC-MS

Urine (0–24 h after intake)

• Tartaric acid

[158]

  Grape pomace beverage (500 mL)

Crossover, placebo-controlled

12 (6 F, 6 M)

LC-MS

Urine

• cis-Resveratrol-3-O-glucuronide,

• cis-Resveratrol-3-O-sulfate,

• cis-Resveratrol-4′′-O-glucuronide,

• cis-Resveratrol- 4-O-sulfate

• trans-Resveratrol-3-O-glucuronide,

• trans-Resveratrol-3-O-sulfate,

• trans-Resveratrol-4′′-O-glucuronide,

• trans-Resveratrol-4-O-sulfate

• Dihydroresveratrol-3-O-sulfate,

• Dihydroresveratrol-4-O-sulfate,

• Dihydroresveratrol-sulfoglucuronide

[150]

  Grape skin extract beverage (187 mL)

Single dose & long-term study (2 weeks), crossover, placebo-controlled

26 (13 F, 13 M)

UPLC MS/MS

Urine: 0–4 h after intake (acute study) and 24-h urine (long-term study)

• trans-Resveratrol-3-O-glucuronide,

• trans-Resveratrol-4′-O-glucuronide,

• trans-Resveratrol-3′-O-sulfate,

• trans-Resveratrol-4′-O-sulfate,

• trans-Resveratrol-3,4′-O-disulfate

• cis-Resveratrol-3-O-glucuronide,

• cis-Resveratrol-4′-O-glucuronide,

• cis-Resveratrol-3′-O-sulfate,

• cis-Resveratrol-4′-O-sulfate

• Resveratrol sulfoglucuronide

• trans and cis-piceid

• Piceid glucuronide,

• Piceid sulfate

• Dihydroresveratrol-3-O-sulfate,

• Dihydroresveratrol-4-O-sulfate,

• Dihydroresveratrol-sulfoglucuronide

[143]

  Grape extract tablets (15 tablets with 400 mL of water)

Single-dose study, parallel design

3 M

LC–ESI-MS/MS

Plasma (0–48 h after intake)

Urine (0–48 h after intake)

• trans-Resveratrol-3-O-glucuronide (u, p),

• trans-Resveratrol-4′-O-glucuronide (u, p),

• trans-Resveratrol-3-O-sulfate (u),

• trans-Resveratrol-4′-O-sulfate (u)

• cis-Resveratrol-3-O-glucuronide (u, p),

• cis-Resveratrol-4′-O-glucuronide (u, p) ,

• cis-Resveratrol-3-O-sulfate (u),

• cis-Resveratrol-4′-O-sulfate (u)

• trans- and cis-piceid (u)

• piceid-glucuronide (u, p),

• piceid sulfate (u)

• Dihydroresveratrol-glucuronide (u, p),

• Dihydroresveratrol-sulfate (u)

[142]

  Resveratrol (250 mg), grape seed extract (900 mg) vs grape juice (20 oz)

Pharmacokinetic challenge, 10 days with repeated doses

7 M, 5 F

LC-MSMS

Blood: 0.5 h, 1 h, 1.5 h, 2 h, 2.5 h, 3 h, 4 h, 5 h, 6 h

• Resveratrol

[117]

Blueberry

  Bluberry extract 25 g, single-dose kinetic study

Single-dose study

10

LC-ESI-MS-

Orbitrap

Untargeted study

Serum: 30, 60, 120, 240, and 360 min

Urine: 30, 60, 120, 240 and 360 min

• Delphinidin hexoside (u)*

• Cyanidin hexoside (u)*

[2]

  300 g of blanched vs unblanched blueberries

Randomized crossover design

10 M

HPLC-UV

Blood plasma: 0 h, 1 h. 2 h, 24 h

• Malvidin-3-glucoside (p)

• Cyanidin-3-glucoside (p)

• Phenyl-γ-valerolactone metabolite

[37]

  Blueberry 250 mL juice

Single-dose kinetic study

17 (13 F, 4 M)

HPLC-ESI-MS/MS

Urine: 0 h, every void during 24 h

• Cyanidin metabolites (including glucuronide and methyl glucuronide)

• Pelargonidin metabolites

• Delphinidin (including glucuronide and methyl glucuronide)

• Malvidin (including glucuronide and methyl glucuronide)

• Peonidine (including glucuronide and methyl glucuronide)

• Petunidin (including glucuronide and methyl glucuronide)

[81]

  250 mL of blueberry juice per day, for 28 days (216 mg (448 μmol) cyn 3-glucoside)

Randomized one-arm study

17 (13 F, 4 M)

HPLC-ESI-MS/MS

Urine 24 h: days 0, 7th, 14th, 28th, and 36th

• Cyanidin glucuronide

• Delphinidin glucuronide

• Malvidin arabinose

• Malvidin glucuronide

• Malvidin glycoside

• Malvidin methyl glucuronide

• Pelargonidin glucuronide

• Pelargonidin methyl glucuronide

• Pelargonidin methyl glycoside

• Peonidin glucuronide

• Peonidin glycoside

• Peonidin methyl glucuronide

• Petunidin

• Petunidin glucuronide

• Petunidin methyl glucuronide

[83]

  Blueberry powder in combination with placebo oil and fish oil. Powder dose corresponded to 25g fresh fruit

Randomized, double blind, parallel groups, placebo-controlled trial

76

HPLC-MS

Urine, morning samples, after overnight fasting, day 0, day 12th

• Total antocyanins including glucuronide conjugates

[106]

  blueberry 100g (containing 1.2 g antocyanins)

Single-blind crossover with control meal

5 (not specified)

HPLC-UV

Blood serum: 0 h, 1 h, 2 h, 3 h, 4 h

• Cyanidin-3-glycosides

• Delphinidin-3-glycosides

• Malvidin-3-glycosides

• Petunidin-3-glycosides

[103]

  300 mL blueberry extract

Single-dose crossover

5 M

HPLC-UV

Urine: 0 h, 60 min, 120 min, 180 min, 240 min, 300 min

• Cyanidin-3-glycosides

• Delphinidin-3-glycosides

• Malvidin-3-glycosides

• Petunidin-3-glycosides

[105]

  10 g bilberry extract

Single dose

10 F

HPLC-MS/MS

Urine: 0–2 h, 2–4 h, 4–8 h,

Blood: 0–2 h, 2–4 h, 4–8 h, 8–24 h

Ileostomy fluid: 0–1 h, 1–2 h, 2–4 h, 4–6 h, 6–8 h

• Malvidin glucuronide

• Peonidin glucuronide

[112]

  189g frozen blueberry blended with 315ml water

Parallel randomized study

5 F

HPLC-DAD

Blood plasma 10 min, 20 min, 30min, 45 min, 1 h, 2 h, 4 h, 6 h, and 24 h postprandial

Urine: 0 h, 0–2 h, 2–4 h, 4–6 h, 6–8 h, 8–12 h, 12–24 h

• Cyanidin-3-glycosides

• Cyanidin-3-glucoside monoglucuronide

• Delphinidin-3-glycosides

• Malvidin-3-glycosides

• Petunidin-3-glycosides

[178]

  25 g freeze dried wild blueberry powder

Single blind, randomized, two-arm crossover-controlled study

6 M, 6 F

UHPLC-Q-TOF-MS2;

UHPLC-QQQ-MS2

Blood: 0.25 h, 0.5 h, 1 h, 2 h, 4 h, 6 h, 8 h, 10 h, 24 h fasting

• Malvidin-3-(6′′-acetyl-glucoside)

• Chlorogenic acid

• Cyanidin 3-arabinose

• Cyanidin-3-galactoside

• Cyanidin-3-glucoside

• Cyanidin glucuronide

• Delphinidin-3-arabinose

• Delphinidin-3-galactoside

• Delphinidin-3-glucoside

• Delphinidin glucuronide

• Malvidin-3-arabinose

• Malvidin-3-galactoside

• Malvidin-3-glucoside

• Peonidin-3-arabinose

• Peonidin-3-galactoside

• Peonidin-3-glucoside

• Peonidin glucuronide

• Petunidin-3-arabinose

• Petunidin-3-galactoside

• Petunidin-3-glucoside

• Petunidin glucuronide

[185]

Strawberry

  300 g Fresh strawberries (fs) and stored strawberries (ss)

Single-dose,crossover

13 (not specified)

LC-MS/MS

Blood plasma: 0.5, 1, 2, 3, 5, and 8 h

Urine: 0–2, 2–4, 4–6, 6–8, 8–12, and 12–24 h

• Pelargonidin (u)

• Pelargonidin glucoside (u)

• Pelargonidin glucuronide (u)

[4];

  Strawberry powder: 10 g, 20 g, 40 g

Single-center, randomized, single-blind, four-arm, crossover

5 (not specified)

Q-TOF LC/MS and LC-MS/MS

Blood plasma: 0 h, 30 min, 60 min, 90 min, 120 min, 180 min, 240min, 300 min, 360 min

• Pelargonidin-O-glucuronide

• Pelargonidin sulfate

• Pelargonidin glycosides

• Cyanidin glycosides

[5]

  50 g Daily of freeze-dried strawberry powder for 4 weeks

4-week one-arm study

16 F

HPLC-UV

Fasting serum and plasma

• Ellagic acid

[9]

  500 g Strawberries: integrated food production vs organic production

Open-label crossover design with run-in and washout periods and consisted of 8 visits at the 0th, 10th, 25th, 40th, 50th, 65th, 80th, and 90th day of observation

33 (16 M; 17 F)

HPLC-UV/VIS, HPLC-ECD

Fasting plasma and spot morning urine

• Urolithin A

[14]

  Strawberry juice, 55 g of fruits

Single-intake study

3 M, 3 F

HPLC-MS

Urine: 2 h, 4 h, 6 h, 8 h, and 24 h

• Pelargonidin-3-glucoside

• Pelargonidin-3-rutinoside

• Pelargonidin glucuronide

[20]

  Strawberry puree 100 g, 200 g, 400 g

Dose–response crossover study dosing

12 (not specified)

HPLC-UV-MS

Urine: 0, 2, 4 ,6, 8, 10, 12, and 24 h

• Pelargonidin-3-glucoside

• Pelargonidin glucuronide (3 isomers)

[22]

  250 g Strawberry

Randomized, 4-arm, not crossover.

40 (20 M, 20 F)

LC-MS/MS

Urine: 8, 16, 32, 40, and 56 h

• Urolithin B

• Urolithin B glucuronide

[25, 26]

  Strawberries (150g)

Randomized, controlled, single-blinded, three-way crossover

16 M (overweight, healthy)

LC-ESI- Q-TOF-MS

Urine: 0 h, 0–1 h, 1–2 h, 2–24 h

• Non-specific metabolites of flavonols

• Furaneol glucuronide*

• Furaneol sulfate*

• Mesifurane sulfate*

[31]

  Strawberry 10 g dry powder

Single-centre, randomized, single-blind, placebo controlled,

crossover

24 overweight adults (14 F, 10 M)

LC-MS/MS

Blood plasma: 0, 30, 60, 90, 120, 180, 240, 300, 360 min

• Pelargodnidin sulfate

• Pelargonidin-3-glucoside

• Pelargonidin-3-glucuronide

[41]

  200 g strawberries (179 mol pelargonidin-3-glucoside)

Single dose, dose–response study

6 (3 F, 3 M)

HPLC-ESI-MS-MS, and HPLC-UV

Urine: 0–2, 2–4, 4–6, 6–8, 8–12, and 12–24 h

• Pelagonidin monglucuronide (3 isomers)

• Pelargonidin

• Pelargonidin monosulfate

• Pelargonidin-3-glucoside

[48]

  Frozen strawberries (250 g)

3 weeks intervention, one arm

21 F

LC-MS/MS

Blood plasma and urine

(morning urine, 0–12 h, 12–24 h, washout urine)

• 2,5-dimethyl-4-hydroxy-3-[2H]furanone glucuronide (furaneol glucuronide) (p, u)

• Pelargonidin-glucuronide (3 isomers) (p, u)

• Pelargonidin-3-glucoside (p)

• Urolithin A glucuronide (p, u)

[74];

  100 g, 200 g, 300 g, or 400 g portion of fresh strawberries

Randomized four phase crossover design, dose-response

10 (3M, 7F)

HPLC-UV-MS

Urine: 0–2, 2–4, 4–6, 6–8, and 8–24 h

• Pelagonidin monglucuronide (3 isomers)

• Pelargonidin

• Pelargonidin monosulfate

• Pelargonidin-3-glucoside

[75, 76];

  200 g of strawberries, containing 222 μmol of pelargonidin-3-O-glucoside

Single-dose, crossover study. Treatment vs control

8 (6 M, 2 F)

HPLC-PDA-MS2

Blood plasma (0, 0.5, 1, 2, 3, 4, 6, 8, and 24 h) and

urine (0–2, 2–5, 5–8, and 8–24 h)

• Pelargonidin-glucuronide (4 isomers) (p, u)

• Pelargonidin-3-O-glucoside (p, u)

• Pelargonidin-O-monosulfate (u)

• Pelargonidin (u)

[113]

  Dry strawberry powder: 10 g, 20 g, 40 g, and placebo 0 g

A randomized, single-center, single-blinded, four-arm, placebo-controlled, 6-h postprandial, crossover study

25 (not specified)

HPLC-Triple Quandrupole MS

Blood plasma 0, 30, 60, 90, 120, 180, 240, 300, and 360 min,

• Pelargonidin-3-O-glucoside

• Pelargonidin glucuronide

• Cyanidin-3-O-glucoside

[126]

  500 g Daily strawberry consumption for 9 days

Open label, treatment vs control with a run-in and wash-out period, consisted of 7 visits

14 (not specified)

HPLC-UV/VIS, HPLC-ECD

Fasting plasma and spot morning urine

• Urolithin A

[129]

  2.5 kg Spanish strawberry and 3.0  kg Italian strawberry

Two groups, parallel, not crossover

6 (4 M, 2 F)

LC-ESI-MS/MS

Urine: 24 h

• 2,5 dimethyl-4-hydroxy-3[2H]furanone

• 2,5 dimethyl-4-hydroxy-3[2H]furanone glucuronide

[141]

  Strawberry drink: 132 g of fresh strawberries (34.7 ± 0.5 mg anthocyanins per drink)

Within-subjects crossover design, delivering one strawberry drink and two control drinks

24 (not specified)

UPLC-Triple Quandrupole MS

Blood plasma, from 0 to 10 h after meal

• Pelargonidin-3-O-glucoside

• Pelargonidin glucuronide

• Pelargonidin-3-O-rutinoside

• Cyanidin-3-O-glucoside

• Cyanidin-3-O-rutinoside

[147]

  12 g of freeze-dried strawberry powder

Double-blinded, 2-arm, placebo-controlled

90-day feeding trial

38

LC-MS/MS

Blood:

Day 1 fasting blood;

Day 45: fasting blood and 2 h postprandial

Day 90: fasting blood and 2 h postprandial

• Urolithin A glucuronide

• Isourolithin A glucuronide

• Urolithin B glucuronide

• Pelargonidin-3-glucoside

• Pelargonidin-3-rutinoside

• Pelargonidin glucuronide

[148]

  200 g of fresh strawberries or 200 g strawberry puree

4-week randomized study

20 (8 M, 12 F)

LC-MS/MS

Urine: 0−8, 8−32, 32−56, 56−80, and 80−92 h

• Urolithin A glucuronide

• Urolithin A

• Urolithin B

• Urolithin B glucuronide

[165]

  Strawberry milk beverage and strawberry water beverage; 12 g of powder in each drink

Single-center, randomized, single-blinded, crossover study

9

 

Blood 0 h, 0.25 h, 0.5 h, 1 h, 1.5 h, 2 h, 3 h, 4 h, 5 h, 6 h

• Pelargonidin-3-glucoside

• Pelargonidin-3-rutinoside

• Pelargonidin glucuronide

[179]

Raspberry

  300 g of raspberries

Acute, 1-arm study

10 healthy persons (6 M, 4 F); 4 with ileostomy

HPLC-PDA-MS2

Blood plasma: 0, 1.0, 1.5, 2.0, 3.0, 5.0, 6.5, 7.5, and 24  h

Urine: 0–4 h, 4–7 h, 7–24 h, 24–32 h, and 32–48 h

Ileal fluid: 0–4 h, 4–7 h, 7–24 h, and 24–48 h

• Cyanidin-3-O-(2′′-O-glucosyl)rutinoside (if, u)

• Cyanidin-3-O-(2′′-O-xylosyl)rutinoside (if)

• Cyanidin-3-O-glucoside (if, u)

• Cyanidin-3-O-rutinoside (if)

• Cyanidin-3-O-sophoroside (if, u)

• Ellagic acid(if, u)

• Ellagic acid-O-glucuronide (u)

• Pelargonidin-3-O-(2′′-O-glucosyl)rutinoside (if)

• Pelargonidin-3-O-glucoside (if)

• Pelargonidin-3-O-sophoroside (if)

• Sanguiin H-6 (if)

• Urolithin A glucuronide (u)

[70]

  200 g, 400 g of raspberries, + placebo

3-arm double-blind randomized controlled crossover

10 M

UPLC-QTOF

Blood: 0 h, 2 h and 24 h postprandial

• Urolithin A

• Urolithin A-3-glucuronide

• Urolithin A-sulfate

• Urolithin B glucuronide

• (Iso)urolithin A

• (Iso)urolithin A-3-glucuronide

[78]

  300 g of homogenized raspberries

Acute, single dose

9 (4 M, 5 F)

UHPLC-MSn and UHPLC-MS2

Urine: 0–4 h, 4–8 h, 8–24 h, 24–32 h, 32–48 h

Blood plasma: 0.5 h, 1 h, 1.5 h, 2 h, 3 h, 4 h, 5 h, 6 h, 8 h, 24 h

• (Iso)urolithin A-sulfate-O-glucuronide (u, p)

• Isourolithin A-O-glucuronide (u, p)

• Peonidin-3-O-glucoside (u)

• Urolithin A (u)

• Urolithin A-O-glucuronide (u, p)

• Urolithin A-sulfate (u, p)

• Urolithin B (u)

• Urolithin B-3-O-glucuronide (u, p)

• Dimethylellagic acid-O-glucuronide (u, p)

• Cyanidin-3-O-glucoside (u, p)

• Cyanidin-3-O-glucuronide (p)

• Peonidin-3-O-glucoside (u)

[98]

  Intragastric dosage of raspberry ketone, 1 mmol/kg

Single dose

(not specified)

GC-MS after derivatization

Urine of rat,rabbit, and guinea pig

• 2-(4-hydroxyphenyl)ethanol

• 4-(4-hydroxyphenpl)butan-2-one

• 4-hydroxybenzoic acid

• 4-hydroxyphenylacetic acid

• 4-(4-hydroxyphenyl)butan-2-ol

• 4-(4-hydroxy-3-methoxyphenyl)butan-2-one

• 4-hydroxy-4-(4-hydroxyphenyl)butan-2-one

• 3-(4-hydroxyphenyl)propionic acid

• 4-(3,4-dihydroxyphenyl)butan-2-one

• 4-(4-hydroxy-3-methoxpphenyl)butan-2-ol

• 4-(4-hydroxyphenyl)butan-2,3-diol

• 4-(3,4-dihydroxyphenyl)butan-2-ol

• 1-hydroxy-4-(4-hydroxphenyl)butan-2-one

• 4-(4-hydroxyphenyl)butan-l,2-diol

[156]

  125 g raspberries per day for 4 weeks.

Not specified

3

UHPLC-QTOF (MS/MS);

UHPLC-QQQ (MS/MS)

Blood: 0 h, 0.5 h, 1 h, 2 h, 3 h, 4 h, 5 h, 5.5 h, 6 h, 7 h, 8 h, and 24 h

Urine: − 12 h–0 h; 0–4 h, 4–8 h, 8–24 h, 24–36 h, 36–48 h

• Cyanidin-3-O-sophoroside

• Cyanidin-3-O-(2G glucosylrutinoside)

• Cyanidin-3-O-glucoside

• Pelargonidin-3-O-sophoroside

• Cyanidin-3-O-rutinoside

• Cyanidin-3-O-glucuronide

• Methyl cyanidin-3-O-sophoroside

• Peonidin-3-O-glucoside

• Urolithin A glucuronide

• Urolithin B glucuronide

• Urolithin A

[184]

Blackberry

  200 g of blackberries (containing 960 μmol of anthocyanins expressed as cyanidin 3-glucoside equivalents)

Acute, single dose, kinetic study

5 (3 F, 2 M)

HPLC-ESI-MS-MS and HPLC with UV-vis

Urine: 0–2, 2–4, 4–6, 6–8, 8–12, and 12–24 h

• Cyanidin glycosides

• Cyanidin glucuronide

• Cyanidin diglucuronide

• Cyanidin sulfate

• Peonidin glycosides

• Peonidin glucuronide,

• Peonidin-3-glucoside glucuronide

[47]

  250 mL of tropical highland blackberry juice

Acute study, repeated over the year, no placebo, different kinetics design

26 (16 F, 10 M)

UPLC-DAD/ESI-Q-TOF/MS2

Spot urine samples

• Urolithin A

• Urolithin B

• Urolithin C

• Urolithin D

• Urolithin M5

• Methyl urolithin A

• Urolithin glucuronide A

• Urolithin glucuronide B

• Urolithin glucuronide C

• Urolithin glucuronide D

• Ellagic acid

• Ellagic acid dimethyl ether glucuronide

• Ellagic acid dimethyl ether

[64, 65]

  Freeze-dried blackberries: 32 g for females and 45 g for males

26 weeks pilot study with daily consumption of supplement

20

LC-MS/MS

3 h pooled urine collected in the morning: week 0, week 12, week 26

• Urolithin A glucuronide

• Urolithin A-sulfate

• Dimethylellagic acid glucuronide

[89]

  250 g of blackberries

Randomized and crossover intervention

18 (not specified)

HPLC-DAD

Blood plasma: 15, 30, 60, and 12 min

Urine: 0, 120 min

• Cyanidin glycosides (u)

• Cyanidin glucoside glucuronide (u, p)

• Cyanidin glucoside sulfate (p, u)

• Cyanidin glucuronide (two isomers) (p, u)

• Methyl cyanidin glucoside glucuronide (p, u)

• Methyl cyanidin glucuronide (p, u)

[100]

  20 g freeze-dried blackberry powder, three times a day, for 9 weeks

One-arm study, patients with colorectal cancer

20 (17 M, 3 F)

UHPLC-MS/MS, Orbitrap LTQ, and GC-MS

Blood plasma, urine at baseline and after treatment

• Cyanidin glycosides (u)

[123]

  45 g of freeze-dried blackberries

One arm, 1 week study with 45 g of meal daily

10 M

LC-MS/UV-Vis; HPLC-ESI-MS/MS

Urine: 4 h, 8 h, 12 h, at 1st and 7th day

• Cyanidin glycosides

[161]

Cranberry

  480 mL cranberry

Juice

Acute, single-dose, kinetic study

15 (13 M, 2 F)

LC-Diode array/ ion trap MS/MS

Blood plasma: 0 h, 1 h, 2 h,  h, 4 h

urine: 0–4 h

• Cyanidin-3-glycosides (u, p)

• Malvidine-3-glycosides (u, p)

• Peonidin-3-glycosides (u, p)

[108];

  200 mL cranberry juice

Acute, single-dose, kinetic study

11 (9 M, 2 F)

HPLC-ESI-MS-MS

Urine 24 h

• Cyanidin-3-glycosides

• Malvidine-3-glycosides

• Peonidin-3-glycosides

[119]

  250 mL cranberry juice twice a day

Crossover, 2-arm study

17 F

UHPLC-Q-Orbitrap-HRMS

Blood: fasting base line, 2h postprandial on third consumption day

• 5-(trihydroxphenyl)-γ-valerolactone*

• Phenolics derivatives*

[94]

  450 mL

Double-blind, placebo-controlled parallel trial

78

LC-MS/MS

Urine: 0 h, 3 h, 5 h, 8h postprandial

• Cyanidin-3-glucoside

• Peonidin-3-glucoside

• Cyanidin-3-galactoside

• Peonidin-3-galactoside

• Peonidin-3-arabinoside

• Cyanidin-3-arabinoside

[27]

  2 types of capsules of cranberry extract, intake for 7 days; 36 mg vs 12 mg extract per capsule

Randomized, double-blind, 2-arm repeated measure crossover design

13

LC-LTQ-Orbitrap XL

Urine: 0 h, 1 h, 2 h, 4 h, 6 h, 10 h, 12 h, 24 h, at day 0 and day 7th

• Hydroxyphenyl-valerolactone derivatives*

[7]

Blackcurrant

  100 g whole blackcurrant vs 50 g diluted blackcurrant syrup

Randomized two-phase crossover

10 (3 M, 7 F)

HPLC-ESI-MS

Blood plasma: 15 min, 30 min, 45 min and 1 h, 1.5 h, 2 h, 3 h, 4 h, 6 h, 8 h, 24 h, and 48 h

Urine: 0–2 h, 2–4 h, 4–6 h, 6–8 h, 8–24 h and 24–48 h

• Cyanidin-3-O-rutinoside (u)

• Delphinidin 3-O-rutinoside (u)

[75, 76]

  250 mL black currant juice vs placebo drink

Randomized, cross-over, double-blind, placebo-controlled acute meal study

20 (11 F, 9 M)

GC-MS

urine: collected every 2 h and at 24 h

• Cyanidin-3-O-rutinoside

• Delphinidin 3-O-glucoside

• Delphinidin 3-O-rutinoside

[80]

  300 mL blackcurrant extract

Acute crossover

5 M

HPLC-UV

Urine: 0 h, 60 min, 120 min, 180 min, 240 min, 300 min

• Cyanidin-3-O-rutinoside

• Cyanidin-3-O-glucoside

• Delphinidin 3-O-glucoside

• Delphinidin 3-O-rutinoside

[105]

  253 mg of blackcurrant extracts

Acute single dose

4 (3 F, 1 M)

LC-MS/MS

Blood plasma: 0 h, 0.5 h, 1 h, 2 h, 3 h, 4 h, 6 h

• Cyanidin-3-O-rutinoside

• Cyanidin-3-O-rutinoside

• Delphinidin 3-O-glucoside

• Delphinidin 3-O-rutinoside

[114]

  200 mL blackcurrant juice

Acute, single-dose, kinetic study

4 (2 M , 2 F)

HPLC-UV-VIS

Urine: 0 h, 0.5 h, 1 h, 1.5 h, 2 h, 2.5 h, 3 h, 3.5 h, 4 h, 4.5 h, 5 h

• Cyanidin-3-O-rutinoside

• Cyanidin-3-O-glucoside

• Delphinidin 3-O-glucoside

• Delphinidin 3-O-rutinoside

[115]

  1.6 g blackcurrant extract powder in 200 mL water

Acute single-dose kinetic study

5 M

HPLC-ESI-MS/MS

Plasma 0 h, 1 h, 2 h, 4 h, 6 h, 8 h

Urine: 24−0 h prior to ingestion; 0−2 h, 2−4 h, 4−6 h, 6−8 h, 8−12 h, 12−24 h,

24−48 h postprandial

• Delphinidin 3-O-rutinoside

• Delphinidin 3-O-glucuronide

• Cyanidin-3-O-glucoside

• Cyanidin 3-O-glucuronide

[139]

  1. * Metabolites found through untargeted metabolomics experiments
  2. u urine, p plasma, if illeal fluid