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  • New procedure of selected biogenic amines determination in wine samples by HPLC.

New procedure of selected biogenic amines determination in wine samples by HPLC.

Analytica chimica acta (2014-06-15)
Anna M Piasta, Aneta Jastrzębska, Marek P Krzemiński, Tadeusz M Muzioł, Edward Szłyk
ABSTRACT

A new procedure for determination of biogenic amines (BA): histamine, phenethylamine, tyramine and tryptamine, based on the derivatization reaction with 2-chloro-1,3-dinitro-5-(trifluoromethyl)-benzene (CNBF), is proposed. The amines derivatives with CNBF were isolated and characterized by X-ray crystallography and (1)H, (13)C, (19)F NMR spectroscopy in solution. The novelty of the procedure is based on the pure and well-characterized products of the amines derivatization reaction. The method was applied for the simultaneous analysis of the above mentioned biogenic amines in wine samples by the reversed phase-high performance liquid chromatography. The procedure revealed correlation coefficients (R(2)) between 0.9997 and 0.9999, and linear range: 0.10-9.00 mg L(-1) (histamine); 0.10-9.36 mg L(-1) (tyramine); 0.09-8.64 mg L(-1) (tryptamine) and 0.10-8.64 mg L(-1) (phenethylamine), whereas accuracy was 97%-102% (recovery test). Detection limit of biogenic amines in wine samples was 0.02-0.03 mg L(-1), whereas quantification limit ranged 0.05-0.10 mg L(-1). The variation coefficients for the analyzed amines ranged between 0.49% and 3.92%. Obtained BA derivatives enhanced separation the analytes on chromatograms due to the inhibition of hydrolysis reaction and the reduction of by-products formation.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Chloroform-d, 99.8 atom % D, contains 0.03 % (v/v) TMS
Sigma-Aldrich
Chloroform-d, "100%", 99.96 atom % D, contains 0.03 % (v/v) TMS
Sigma-Aldrich
Tryptamine hydrochloride, 99%
Sigma-Aldrich
Phenethylamine, purified by redistillation, ≥99.5%
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Chloroform-d, 99.8 atom % D, contains 1 % (v/v) TMS
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, 99.93%
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Chloroform-d, ≥99.8 atom % D, anhydrous
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Chloroform-d, "100%", 99.95 atom % D
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Chloroform-d, 99.8 atom % D, contains 0.05 % (v/v) TMS
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N-Ethyldiisopropylamine solution, suitable for peptide synthesis, ~2 M in 1-methyl-2-pyrrolidinone
Supelco
Methanol, analytical standard
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Sodium hydroxide solution, BioUltra, for molecular biology, 10 M in H2O
Sigma-Aldrich
Sodium hydroxide, BioUltra, for luminescence, ≥98.0% (T), pellets
Supelco
Sodium hydroxide solution, 49-51% in water, eluent for IC
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Phenethylamine, ≥99%
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N-Benzylmethylamine, 97%
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3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
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Chloroform-d, ≥99.8 atom % D, contains 0.5 wt. % silver foil as stabilizer, 0.03 % (v/v) TMS
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Phenethylamine, 99%
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Chloroform-d, 99.8 atom % D, contains 0.1 % (v/v) TMS
Sigma-Aldrich
Chloroform-d, 99.8 atom % D
Sigma-Aldrich
Chloroform-d, "100%", 99.96 atom % D, contains 0.5 wt. % silver wire as stabilizer
Sigma-Aldrich
Chloroform-d, ≥99.8 atom % D, contains 0.5 wt. % silver foil as stabilizer
Sigma-Aldrich
Methanol, anhydrous, 99.8%
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Sodium hydroxide solution, 1.0 N, BioReagent, suitable for cell culture
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Tyramine hydrochloride, ≥98%
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Sodium hydroxide solution, 7 M
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N-Ethyldiisopropylamine, BASF quality, ≥98.0%
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Methanol, SAJ special grade
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Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC