Determination of biogenic amines in fresh and processed meat by suppressed ion chromatography-mass spectrometry using a cation-exchange column (original) (raw)

Determination of biogenic amines in fresh and processed meat by ion chromatography and integrated pulsed amperometric detection on Au electrode

Food Chemistry, 2007

A new method for simultaneous determination of underivatized biogenic amines based on the separation by cation-exchange chromatography and suppressed conductivity coupled with mass spectrometry detection has been developed. The method has been applied to the analysis of cadaverine, putrescine, histamine, agmatine, phenethylamine and spermidine in processed meat products. The amines were extracted from muscle tissue with methanesulfonic acid without any additional derivative step or sample clean-up. Biogenic amines were separated by the IonPac CS17 column, a cation-exchange column used with gradient elution, and detection was done by suppressed conductivity and mass spectrometry. Tyramine was simultaneously analysed by using a spectrophotometer (275 nm) before the suppressed conductivity detection. Linearity of response was obtained in the range 0.25-25 g mL −1 . The detection limits ranged from 23 g L −1 for putrescine to 155 g L −1 for spermidine (suppressed conductivity) and from 9 g L −1 for agmatine to 34 g L −1 for spermidine (MS). Average recoveries from meat samples ranged from 85 to 97% and coefficients of variation ranged from 4.5 to 9.7%. The analysis of biogenic amines in fresh and processed meats (dry-cured, cooked and fermented products) can be used as a quality marker of raw material and for studying the relationship between their changes and the fermentation process involved in dry sausage ripening.

Simultaneous determination of ten underivatized biogenic amines in meat by liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)

Journal of Mass Spectrometry, 2014

Biogenic amines (BAs) are considered to be important indicators of freshness and quality in food. In this work, an analytical method for analyzing ten underivatized BAs in meat by performance liquid chromatography-tandem mass spectrometry has been developed. Comparison between ion trap and triple quadrupole as mass analyzers indicated that the latter provides greater sensitivity and selectivity. The range of the correlation coefficients of the calibration curves of the analyzed compounds was 0.987-0.999, and the limits of detection and limits of quantification were in the range of 0.002-0.1 mg l À1 and 0.008-0.5 mg l À1 , respectively. Once validated, the method was used to analyze the concentrations of BAs in 16 commercial meat samples, for evaluating the freshness of food through the study of BA indices, i.e. biogenic amine index (BAI) and the ratio spermidine/spermine (SPD/SPE). The results indicated that all the samples were fresh, with a BAI lower than 1.49 mg kg À1 and a SPD/SPE ratio lower than 0.41 in each case. This methodology for testing the freshness of meat has potential for quality control applications along the entire production chain of meat products.

A comparative study for determination of biogenic amines in meat samples by capillary isotachophoresis with two electrolyte systems

European Food Research and Technology, 2012

The selected biogenic amines, BAs (putrescine, cadaverine, histamine, tyramine, spermidine and spermine), in pork, beef, and poultry meat samples were determined by two simple procedures without derivatization using isotachophoretic technique. Two electrolyte systems were proposed for their separation and determination with satisfactory separation parameters. The linearity of the proposed procedures was between 2-10 mg L-1 and 5-50 or 10-60 mg L-1 , whereas average recoveries for the standard solutions of amines and their mixture varied between 99-100 % and 95-105 %, respectively. Average recoveries for standard addition method (96-99 %) indicated satisfactory accuracy of proposed electrolyte systems. The obtained coefficient of variation values for standard solutions and meat samples ranged from 0.62 to 4.54 % and from 0.56 to 6.03 %, respectively, which confirmed good repeatability. Except for spermidine and spermine, BAs levels in fresh meat samples were generally low. The effect of storage time on the content of biogenic amines in meat was also studied indicating the increase of BAs levels (excluding Spermine and Spermidine).

Validation of an HPLC Methodology for the Identification and Quantification of Biogenic Amines in Chicken Meat

Food Analytical Methods, 2013

This study validated a high performance liquid chromatography (HPLC) method to determine biogenic amines in chicken meat. For the identification of biogenic amines, an isocratic elution system coupled with a UV detector (254 nm) was used after a perchloric acid (5 %) extraction and benzoyl chloride derivatization of the samples. The standards of tyramine, putrescine, cadaverine, spermidine, and spermine were used for the following validation parameters: selectivity, linearity, accuracy, recovery, limit of detection and quantification, and robustness. Finally, chicken meat commercialized in two types of packaging was evaluated. The results showed an excellent selectivity and separation of all amines, r 2 >0.99, relative standard deviation <5 %, recovery between 64 and 112 %, limits of detection and quantification between 0.03-1.25 and 0.15-5.00 μgL −1 , respectively, and appropriate robustness for the proposed methodology. Moreover, both chicken meat commercial packages had similar values for all amines; only tyramine was significantly different (P≤0.05). The proposed method was suitable to detection and quantification of simultaneous five biogenic amines in chicken meat.

Determination of biogenic amines in food samples using derivatization followed by liquid chromatography/mass spectrometry

Analytical and Bioanalytical Chemistry, 2009

A liquid chromatography (LC)/mass spectrometry method was developed for the determination of selected biogenic amines in various fish and other food samples. It is based on a precolumn derivatization of the amines with succinimidylferrocenyl propionate under formation of the respective amides and their reversed-phase liquid-chromatographic separation with subsequent electrospray ionization mass-spectrometric detection. Deuterated putescine, cadaverine, and histamine are added prior to the derivatization as internal standards that are coeluted, thus allowing excellent reproducibility of the analysis to be achieved. Depending on the analyte, the limits of detection were between 1.2 and 19.0 mg/kg, covering between 2 and 3 decades of linearity. The limit of detection and the linear range for histamine are suitable for the surveillance of the only defined European threshold for biogenic amines in fish samples. Compared with the established ortho-phthalaldehyde (OPA)/LC/fluorescence method, the newly developed method allows an unambiguous identification of the biogenic amines by their mass spectra in addition to only retention times, a fivefold acceleration of the separation, and independency from the sample matrix owing to the isotope-labeled internal standards. Various fish, calamari, and salami samples were successfully analyzed with the new method and validated with an independent OPA/LC/fluorescence method.

Detection of common biogenic amines in fermented sausage produced in Turkey

Data in Brief

The application of HPLC method to detect the BA concentration in fermented sausage was successful and proved that HPLC system and method served its purposes. Biogenic amines are generated in foods as a result of free amino acid decarboxylation by bacterial enzymes. Biogenic amines accumulations are unwanted in all foods and beverages because if consumed at high concentrations, they may induce foodborne intoxications. Histamine, putrescine, cadaverine, tyramine, tryptamine, beta-phenylethylamine, spermine and spermidine are considered to be the most important biogenic amines occurring in foods. The determination of biogenic amines in foods is of great interest due to their potential toxicity and can be used as indicators for food quality markers.

A review of the liquid chromatographic methods for the determination of biogenic amines in foods

Food Chemistry, 2013

Biogenic amines (BAs) are biologically active molecules which have aliphatic (putrescine, cadaverine, spermine, spermidine), aromatic (tyramine, phenylethylamine) or heterocyclic (histamine, tryptamine) structures. They can be detected in raw and processed foods which are formed and degraded through several pathways during the metabolic processes of animals, plants and microorganisms. The identification and quantitation procedures of BAs in food samples are very important, because BAs are considered as the indicators of food quality and freshness. The determination of BAs are commonly achieved by separation techniques such as high-performance liquid chromatography (HPLC), gas chromatography (GC) and capillary electrophoresis (CE). In this article, analysis of BAs in foods were reviewed from 2007 to present.

Analysis of nonpolar heterocyclic amines in cooked foods and meat extracts using gas chromatography–mass spectrometry

Journal of Chromatography A, 1998

Heat processing of muscle foods gives rise to the formation of mutagenic and carcinogenic heterocyclic amines, often at ng / g levels. A gas chromatographic-mass spectrometric (GC-MS) technique was introduced for the analysis of nonpolar heterocyclic amines in common cooked meats, pan residues, and meat extracts after solid-phase extraction. The mutagenic heterocyclic amines 3-amino-1,4-dimethyl-5H-pyrido[4,3-b]indole (Trp-P-1), 3-amino-1-methyl-5H-pyrido[4,3-b]indole (Trp-P-2), 2-amino-9H-pyrido[2,3-b]indole (AaC) and 2-amino-3-methyl-9H-pyrido[2,3-b]indole (MeAaC) were identified in several samples in amounts up to 8 ng / g. Also the comutagenic substances 1-methyl-9H-pyrido [3,4-b]indole (harman) and 9H-pyrido[3,4-b]indole (norharman) were detected in the samples in amounts up to almost 200 ng / g. The GC-MS method can be applied without derivatisation of the sample. The technique offers high chromatographic efficiency, yielding detection limits for pure references in the range 0.1-2 ng per injection.

Comparison of the HPLC and the TLC Techniques for the Determination of Biogenic Amines Spiked to Sausage and Smoked Herring Samples

Enliven: Toxicology & Allied Clinical Pharmacology, 2018

The aim of our study to comparative the suitability of chromatographic techniques such as thin layer chromatography (TLC)-densitometry and high performance liquid chromatography (HPLC) for the analysis of biogenic amines in fish and meat products was carried out. The recovery percent of the tested biogenic amines spiked to sausage and smoked herring samples was 92.0-102.2% and 94.5-100.3 % for HPLC versus 86.2-98.5 % and 88.0- 98.0% for the recommended one-dimensioned TLC, respectively. It could be observed that there were not significant differences in the recovery percentages of tryptamine, β-phenylethylamine, putrescine, histamine and tyramine spiked to either sausage sample or smoked herring sample between the tested two analytical methods. Therefore, the TLC-densitometry was found to be rapid and less expensive. In addition, this method is facile, fast, routine, cost effective and suitable method for the analysis of wide range eight biogenic amines and simultaneous screening of several samples at a time.