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Quantification of 3-MCPD and its mercapturic metabolite in human urine: validation of an LC-MS-MS method and its application in the general population.

Quantification of 3-MCPD and its mercapturic metabolite in human urine: validation of an LC-MS-MS method and its application in the general population.

Analytical and bioanalytical chemistry (2015-04-12)

Roberta Andreoli, Martina Cirlini, Antonio Mutti

ABSTRACT

A new method for the simultaneous quantitative determination in human urine of 3-monochloropropane-1,2-diol (3-MCPD), a toxic food contaminant, and its metabolite, 2,3-dihydroxypropyl mercapturic acid (DHPMA), was developed and validated. After urine dilution, the analytes were separated on an Atlantis®dC18 column and quantified by liquid chromatography-tandem mass spectrometry using isotopically labelled internal standards. The limits of quantification (S/N = 10) were 1.90 and 2.21 μg/L for 3-MCPD and DHPMA, respectively. Intra- and inter-day precision were lower than 6 % for each compound. Matrix effects were evaluated. Due to the high sensitivity and good accuracy of the method, 3-MCPD and DHPMA were found in 67 and 100 % of urine samples of healthy subjects, respectively.

MATERIALS

Product Number

Brand

Product Description

Sigma-Aldrich

Triethylamine, ≥99%

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L-Cysteine hydrochloride, anhydrous, from non-animal source, BioReagent, suitable for cell culture, ≥98.0%

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Triethylamine, ≥99.5%

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Triethylamine, puriss. p.a., ≥99.5% (GC)

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Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)

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Sulfuric acid, 99.999%

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1-Butanol, anhydrous, 99.8%

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Methanol, anhydrous, 99.8%

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Acetone, suitable for HPLC, ≥99.9%

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Acetic acid, ≥99.5%, FCC, FG

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Acetic acid, natural, ≥99.5%, FG

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Triethylamine, for amino acid analysis, ≥99.5% (GC)

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Triethylamine, BioUltra, ≥99.5% (GC)

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Triethylamine, for protein sequence analysis, ampule, ≥99.5% (GC)

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L-Cysteine hydrochloride, Vetec^™, reagent grade, ≥98%

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Acetone, natural, ≥97%

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Acetone, ≥99%, meets FCC analytical specifications

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Acetonitrile solution, contains 10.0% acetone, 0.05% formic acid, 40.0% 2-propanol

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Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC

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Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 5 % (v/v) water, 0.1 % (v/v) formic acid, suitable for HPLC

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Sulfuric acid, AR, ≥98%

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Acetonitrile, electronic grade, 99.999% trace metals basis

Supelco

Methanol solution, contains 0.10 % (v/v) formic acid, UHPLC, suitable for mass spectrometry (MS), ≥99.5%