Determination of alkylresorcinol metabolites in human urine by gas chromatography–mass spectrometry

Marklund, Matti; Landberg, Rikard; Åman, Per; Kamal‐Eldin, Afaf

doi:10.1016/j.jchromb.2010.02.007

Cited by 40 publications

(51 citation statements)

References 25 publications

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“…Plasma coffeederived compounds (caffeine and its metabolites, theophylline, theobromine and paraxanthine, and the polyphenols caffeic acid and its metabolites, dihydrocaffeic acid, ferulic acid, dihydroferulic acid, isoferulic acid, dihydroisoferulic acid, dihydro-3-coumaric acid, 3-(3,4-dimethoxyphenyl)propionic acid, 3,4-dimethylcaffeic acid and 3-coumaric acid) were determined using HPLC and GC-MS [10]. The two main urinary alkylresorcinol metabolites 3,5-dihydroxybenzoic acid (DHBA) and 3-(3,5-dihydroxyphenyl)-propanoic acid (DHPPA) were analysed using GC-MS [22]. Blood atom per cent enrichment of 2 H was measured by GC-MS (Agilent 6890 and 5975, Santa Clara, CA, USA) as previously described [13].…”

Section: Modified Botnia Clampmentioning

confidence: 99%

Low-energy diets differing in fibre, red meat and coffee intake equally improve insulin sensitivity in type 2 diabetes: a randomised feasibility trial

et al. 2014

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Aims/hypothesis Epidemiological studies have found that a diet high in fibre and coffee, but low in red meat, reduces the risk for type 2 diabetes. We tested the hypothesis that these nutritional modifications differentially improve whole-body insulin sensitivity (primary outcome) and secretion. acarbose and known disease duration of ≤5 years. Exclusion criteria were: HbA 1c >75 mmol/mol (9.0%), type 1 or secondary diabetes types and acute or chronic diseases including cancer. Patients taking any medication affecting the immune system or insulin sensitivity, other than metformin, were also excluded. Of 59 patients (randomised using randomisation blocks [four or six patients] with consecutive numbers), 37 (54% female) obese type 2 diabetic patients completed this controlled parallel-group 8-week low-energy dietary intervention. The participants consumed either a diet high in cereal fibre (whole grain wheat/rye: 30-50 g/day) and coffee (≥5 cups/day), and free of red meat (L-RISK, n=17) or a diet low in fibre (≤10 g/day), coffee-free and high in red meat (≥150 g/ day) diet (H-RISK, n=20). Insulin sensitivity and secretion were assessed by hyperinsulinaemic-euglycaemic clamp and intravenous glucose tolerance tests with isotope dilution. Whole-body and organ fat contents were measured by magnetic resonance imaging and spectroscopy. Conclusions/interpretation No evidence of a difference between both low-energy diets was identified. Thus, energy restriction per se seems to be key for improving insulin action in phases of active weight loss in obese type 2 diabetic patients, with a potential improvement of subclinical inflammation with the L-RISK diet. Trial Registration: Clinicaltrials.gov NCT01409330

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Section: Modified Botnia Clampmentioning

confidence: 99%

Low-energy diets differing in fibre, red meat and coffee intake equally improve insulin sensitivity in type 2 diabetes: a randomised feasibility trial

et al. 2014

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“…Three different urine samples from a previous study [20] were processed in quadruplicate using a modification of a previously reported method for determination of DHBA and DHPPA [21]. The procedure comprises enzymatic hydrolysis of conjugated AR metabolites, extraction of the deconjugated compounds by liquid-liquid extraction, purification on SPE columns and derivatization of AR metabolites before quantification by GC-MS.…”

Section: Determination Of Ar Metabolites In Urine Samplesmentioning

confidence: 99%

“…A slightly modified protocol based on a previous method [21] was developed to allow accurate quantification of four novel AR metabolites recently identified (DHPPTA, DHBA-glycine, DHCA and DHCA-amide) along with DHBA and DHPPA in urine samples [17,18]. Enzymatic hydrolysis, extraction and SPE of DHBA and DHPPA have been optimized previously [21], and similar conditions were applied in the present method.…”

Section: Determination Of Ar Metabolites In Urinementioning

confidence: 99%

Determination of alkylresorcinols and their metabolites in biological samples by gas chromatography–mass spectrometry

Wierzbicka

Fránek

et al. 2015

Journal of Chromatography B

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High throughput GC-MS methods for quantification of alkylresorcinols (AR), biomarkers of whole grain wheat and rye intake, in plasma and adipose tissue and their metabolites in urine were developed and optimised. Alkylresorcinols in plasma (200μL) and adipose tissues (10-50mg) were extracted with diethyl ether, whereas main AR metabolites such as DHBA and DHPPA and newly identified metabolites in urine (50μL) were extracted with ethyl acetate after enzymatic deconjugation. All extracts were purified on OASIS-MAX solid phase extraction cartridges. Plasma and adipose tissue sample extracts were then derivatised with trifluoroacetic anhydride and reconstituted in undecane, whereas AR metabolites in urine samples were derivatised with BSTFA+TMCS (99:1, v/v, 100μL). Prepared samples were quantified by GC-MS (EI-SIM). Analysis of all compounds in the different matrices showed good selectivity, sensitivity, linearity, precision (<15% within and between batches), adequate recovery (75-108%), and short total run time (10-12min). The methods developed are applicable to large-scale sample sets such as epidemiological studies.

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“…However, this is yet to be confirmed in a low (predominantly wheat) WG consuming population, such as in the UK. The present study evaluated the validity and reproducibility of 24-h urinary DHBA, DHPPA and AR TOT (DHBA + DHPPA) excretion, as a biomarker of WG intake, in healthy UK adults, using samples from the CRESSIDA study (ISRCTN92382106).DHBA and DHPPA excretion was quantified by a modified GC-MS method (2) , in 24-h urine samples collected from 162 healthy men and women, aged 40-70 y. Samples were collected twice at baseline and once at endpoint, following a 12-wk dietary intervention, in which participants were randomised to follow a diet high in refined cereals (CON) or a diet close to dietary guidelines, with an increased content of WG (DG).…”

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confidence: 99%

“…All data presented for log transformed AR:CR urinary excretion, 2 Correlation assessed by Spearman's Rank Test in comparison to estimated WG intake, 3 Difference between DG and CON treatments at endpoint assessed by ANCOVA adjusted for baseline AR metabolite excretion, gender, BMI and age.…”

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Urinary alkylresorcinol metabolites as a biomarker of dietary wholegrain intake and of compliance in a randomised dietary intervention trial: results from the CRESSIDA Study

et al. 2015

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Alkylresorcinols (AR) are a family of phenolic lipids found in the bran fraction of whole grain (WG) wheat and rye, and absent in refined cereals. The AR metabolites, 3,5-dihydroxybenzoic acid (DHBA) and 3-(3,5-dihydroxyphenyl)-propanoic acid (DHPPA) have been proposed as a biomarker of WG intake, and are quantifiable in both plasma and urine (1) . However, this is yet to be confirmed in a low (predominantly wheat) WG consuming population, such as in the UK. The present study evaluated the validity and reproducibility of 24-h urinary DHBA, DHPPA and AR TOT (DHBA + DHPPA) excretion, as a biomarker of WG intake, in healthy UK adults, using samples from the CRESSIDA study (ISRCTN92382106).DHBA and DHPPA excretion was quantified by a modified GC-MS method (2) , in 24-h urine samples collected from 162 healthy men and women, aged 40-70 y. Samples were collected twice at baseline and once at endpoint, following a 12-wk dietary intervention, in which participants were randomised to follow a diet high in refined cereals (CON) or a diet close to dietary guidelines, with an increased content of WG (DG). Dietary intake was assessed by 4-d food diary. Reproducibility was assessed by intra class correlation coefficient (ICC) between duplicate baseline urine collections. Validity was assessed by Spearman's rank test correlations between baseline 24-h urinary AR metabolite excretion and estimated intake of WG, total fibre and cereal fibre. Completeness of urine collection was assessed using the para-amino benzoic acid recovery method (ADJ), a ratio to creatinine (AR:CR) and without adjustment (UNADJ). All data was log transformed prior to statistical analysis.Moderate to high reproducibility was observed for DHBA (ICC = 0·552-0·620) which was greater than that observed for either DHPPA (ICC = 0·427-0·527) or AR TOT (ICC = 0·488-0·583) and higher than that observed in previously published studies (3) . In terms of validity, significant and moderate associations between 24-h urinary excretion and estimated total fibre, cereal fibre and WG intake were found, with the strongest associations for DHBA. Following a 12-week intervention, endpoint AR metabolite excretion was significantly higher following DG vs. CON. For all AR metabolites, the strongest associations with estimated dietary intakes were for AR:CR, followed by UNADJ, with the weakest associations with ADJ recoveries.These results indicate that all AR metabolites are valid and reproducible biomarkers of WG intake in the adult UK population, where wheat is the primary dietary source of WG. The strongest associations with estimated intake were found for DHBA. By contrast, in Nordic populations, DHPPA was the main predictor of WG intake (3,4) probably because rye is consumed in higher amounts as opposed to wheat in the present study. These data suggest total urinary AR adjusted for creatinine may be a useful biomarker of wholegrain intake.

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Determination of alkylresorcinol metabolites in human urine by gas chromatography–mass spectrometry

Cited by 40 publications

References 25 publications

Low-energy diets differing in fibre, red meat and coffee intake equally improve insulin sensitivity in type 2 diabetes: a randomised feasibility trial

Low-energy diets differing in fibre, red meat and coffee intake equally improve insulin sensitivity in type 2 diabetes: a randomised feasibility trial

Determination of alkylresorcinols and their metabolites in biological samples by gas chromatography–mass spectrometry

Urinary alkylresorcinol metabolites as a biomarker of dietary wholegrain intake and of compliance in a randomised dietary intervention trial: results from the CRESSIDA Study

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