Skip to Content

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%

Sigma-Aldrich

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

Sigma-Aldrich

L-Cysteine hydrochloride, anhydrous, ≥98% (TLC)

Sigma-Aldrich

1-Butanol, for molecular biology, ≥99%

Sigma-Aldrich

L-Cysteine hydrochloride, anhydrous, ≥99.0% (RT)

Sigma-Aldrich

Triethylamine, ≥99.5%

Sigma-Aldrich

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

Sigma-Aldrich

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

Sigma-Aldrich

Sulfuric acid, 99.999%

Sigma-Aldrich

1-Butanol, anhydrous, 99.8%

Sigma-Aldrich

Methanol, anhydrous, 99.8%

Sigma-Aldrich

Acetone, suitable for HPLC, ≥99.9%

Sigma-Aldrich

Acetic acid, ≥99.5%, FCC, FG

Sigma-Aldrich

Acetic acid, natural, ≥99.5%, FG

Sigma-Aldrich

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

Sigma-Aldrich

Triethylamine, BioUltra, ≥99.5% (GC)

Sigma-Aldrich

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

Sigma-Aldrich

Methanol, HPLC Plus, ≥99.9%, poly-coated bottles

Sigma-Aldrich

Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid

Sigma-Aldrich

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

Sigma-Aldrich

Acetic acid-¹²C₂, 99.9 atom % ¹²C

Sigma-Aldrich

Acetone, natural, ≥97%

Sigma-Aldrich

Acetone, ≥99%, meets FCC analytical specifications

Sigma-Aldrich

Triethylamine, ≥99.5%

Sigma-Aldrich

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

Sigma-Aldrich

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

Sigma-Aldrich

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

Sigma-Aldrich

Methanol, NMR reference standard

Sigma-Aldrich

Methanol solution, (Methanol:Dimethyl sulfoxide 1:1 (v/v))

Sigma-Aldrich

Acetonitrile, electronic grade, 99.999% trace metals basis