Improved synthesis methods of standards used for quantitative determination of total isothiocyanates from broccoli in human urine

Kristensen, Mette; Krogholm, Kirstine Suszkiewicz; Frederiksen, Hanne; Duus, Fritz; Cornett, Claus; Bügel, Susanne; Rasmussen, Salka E.

doi:10.1016/j.jchromb.2007.01.022

Cited by 11 publications

(12 citation statements)

References 19 publications

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“…Ethanol was purchased from VWR (Briare, France). 1,3‐Benzodithiole‐2‐thione (BD2T) was prepared and characterized as previously described by Kristensen et al . Ultrapure water was produced by a Synergy UV purification system (Millipore, Molsheim, France).…”

Section: Methodsmentioning

confidence: 99%

Improvement in determination of isothiocyanates using high‐temperature reversed‐phase HPLC

Wilson

Ennahar

Marchioni³

et al. 2012

J of Separation Science

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The largely adopted reversed-phase HPLC analysis of the molecular species of isothiocyanates (ITCs) was performed and showed losses during the chromatographic run with eight ITCs. These losses, which obviously impact the accuracy of quantitative determinations, were due to precipitation in the chromatographic system. At 22°C, they ranged from 5.4% for sulforaphane (SFN) to 11.0% for benzyl-ITC when ITCs were injected at 80 μg mL(-1) , but they were up to three times higher at 1 mg mL(-1) reaching 31.9% for benzyl-ITC. The water solubility of the ITCs was a key determinant of the extent of the measured loss. When the column was heated at 60°C, losses in injected ITCs were reduced, in comparison with 22, 40, and 50°C, by two to ten times depending on the ITC considered. A reversed-phase HPLC method based on column heating was suggested and its quantitative performance was determined. It was then applied to the separation of methylene chloride extracts of various cruciferous vegetables. Ally-ITC, SFN, and iberin in cabbage; SFN and iberin in cauliflower; and allyl-ITC and phenylethyl-ITC in horseradish could be identified and quantified. The obtained results cast doubt on quantitative determinations of ITCs that are carried out at room temperature using reversed-phase HPLC.

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Section: Methodsmentioning

confidence: 99%

Improvement in determination of isothiocyanates using high‐temperature reversed‐phase HPLC

Wilson

Ennahar

Marchioni³

et al. 2012

J of Separation Science

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“…Several studies have quantified the pharmacokinetics of sulforaphane following the consumption of broccoli with either active or inactive myrosinase. Most of these studies have analysed sulforaphane and its thiol metabolites in plasma and urine through a cyclocondensation reaction . While this method is efficient at quantifying total thiols, it is not able to discriminate between free isothiocyanates and individual thiol metabolites, or between different isothiocyanates.…”

Section: Introductionmentioning

confidence: 99%

Isothiocyanate concentrations and interconversion of sulforaphane to erucin in human subjects after consumption of commercial frozen broccoli compared to fresh broccoli

Saha

Hollands

Teucher

et al. 2012

Molecular Nutrition Food Res

118

107

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“…Dichloromethane and ethanol were obtained from VWR (Briare, France). 1,3-benzodithiole-2-thione (BD2T) was prepared and characterized previously in our laboratory according to Kristensen et al [ 17 ]. Ultrapure water was produced by a Synergy UV purification system Millipore (Molsheim, France).…”

Section: Methodsmentioning

confidence: 99%

“…The amount of ITCs injected was compared with those collected after separation with and without precolumn derivatization. Quantification was done by using a previously developed assay where ITCs are allowed to react quantitatively with 1,2-benzenedithiol (BDT) forming a stable cyclic dithiol thione product [ 1 , 17 , 18 ]. ITCs and their derivatives could be detected and identified using their UV and mass spectra.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous Determination of Various Isothiocyanates by RP-LC Following Precolumn Derivatization with Mercaptoethanol

et al. 2011

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Numerous isothiocyanates (ITCs) are poorly soluble in water which causes their precipitation in aqueous mobile phases used in reversed phase liquid chromatography (RP-LC), thus impacting the accuracy of the quantification. By comparing the amounts of ITCs injected and released from the column, losses could be estimated at 5–32% depending on polarities and concentrations. Results could be dramatically improved in terms of separation and quantification using RP-LC with a mercaptoethanol precolumn derivatization aimed at avoiding ITCs precipitation. The cancer chemoprotective allyl-ITC and sulforaphane were found in cabbage extracts at 1.2 and 2.7 μg g−1 fresh weight, respectively.

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Improved synthesis methods of standards used for quantitative determination of total isothiocyanates from broccoli in human urine

Cited by 11 publications

References 19 publications

Improvement in determination of isothiocyanates using high‐temperature reversed‐phase HPLC

Improvement in determination of isothiocyanates using high‐temperature reversed‐phase HPLC

Isothiocyanate concentrations and interconversion of sulforaphane to erucin in human subjects after consumption of commercial frozen broccoli compared to fresh broccoli

Simultaneous Determination of Various Isothiocyanates by RP-LC Following Precolumn Derivatization with Mercaptoethanol

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