Piasta Anna M, Jastrzębska Aneta, Krzemiński Marek P, Muzioł Tadeusz M, Szłyk Edward
Faculty of Chemistry, Nicolaus Copernicus University, Gagarin 7 Street, Toruń 87-100, Poland.
Faculty of Chemistry, Nicolaus Copernicus University, Gagarin 7 Street, Toruń 87-100, Poland.
Anal Chim Acta. 2014 Jun 27;834:58-66. doi: 10.1016/j.aca.2014.05.028. Epub 2014 May 22.
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.
提出了一种基于与2-氯-1,3-二硝基-5-(三氟甲基)苯(CNBF)的衍生化反应测定生物胺(BA)的新方法,所述生物胺包括组胺、苯乙胺、酪胺和色胺。通过X射线晶体学以及溶液中的(1)H、(13)C、(19)F核磁共振光谱对与CNBF形成的胺衍生物进行了分离和表征。该方法的新颖之处在于胺衍生化反应的产物纯净且特征明确。该方法应用于通过反相高效液相色谱同时分析葡萄酒样品中的上述生物胺。该方法的相关系数(R²)在0.9997至0.9999之间,线性范围为:0.10 - 9.00 mg L⁻¹(组胺);0.10 - 9.36 mg L⁻¹(酪胺);0.09 - 8.64 mg L⁻¹(色胺)和0.10 - 8.64 mg L⁻¹(苯乙胺),而准确度为97% - 102%(回收率测试)。葡萄酒样品中生物胺的检测限为0.02 - 0.03 mg L⁻¹,而定量限为0.05 - 0.10 mg L⁻¹。所分析胺的变异系数在0.49%至3.92%之间。由于抑制了水解反应并减少了副产物的形成,所得到的BA衍生物增强了色谱图上分析物的分离效果。