Determination of Biogenic Amines in Fresh Fish and Processed Fish Products Using IC-MS/MS (original) (raw)
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Molecules, 2021
In this study, comparative analyses were carried out with ion chromatography mass-spectrometry (IC-MS/MS) which has no derivatization step, high-performance liquid chromatography (HPLC) technique, as well as two quantitative and two semi-quantitative immunoassays. The results demonstrated that HPLC and quantitative immunoassay methods were well-correlated with IC-MS/MS in determining histamine in various types of fish products. The best correlation was observed with the HistaSure ELISA Fast Track kit (R2 = 0.9903). More than half of the values (68%) obtained by two methods were also statistically similar. The results of semi-quantitative test kits also supported histamine values estimated by quantitative methods, with some exceptions. The best results were found for HistaSure Lateral Flow in supporting the quantitative techniques. Therefore, these methods are found suitable for monitoring histamine in fish products in terms of food safety. Good correlations were also observed HPLC a...
Chromatographia, 1993
A new method based on ion exchange chromatography with integrated pulsed amperometric detection has been developed for simultaneous determination of underivatized biogenic amines and applied to the analysis of cadaverine, putrescine, spermidine, and histamine in fish products. The amines were extracted from fish products with a mixture of 5 % aqueous trichloroacetic acid, 6N hydrochloric acid, and nheptane. The extract was passed through a C18 cartridge and the biogenic amines separated by cation exchange on an IonPac CS10 column using gradient elution. Detection was performed by integrated pulsed amperometry, and resulted in estimated detection limits of 5 ng for putrescine, 12 ng for cadaverine and histamine, and 25 ng for spermidine. The method was linear in the range 0.025 to 5 Isg of injected amine. This method was applied to the analysis of products from fish such as Scombridae and Clupeidae. The average recoveries were greater than 92 %.
Science and Technology Indonesia, 2021
Biogenic amines generally can be found in fish due to amines in fish undergoing a degradation process. According to the United States Food and Drug Administration (FDA), biogenic amines in fish and fish products can cause harm to consumers if consumed more than 50 µg/mL. Thus, it is important to analyze them. Five biogenic amines such as heptylamine, histamine, tyramine, cadaverine and spermidine were extracted using soaking method with methanol 50% (v/v), afterward they were detected in fish and fish products using gas chromatography – flame ionisation detector (GC-FID) and the biogenic amines structures were confirmed using mass spectrometry (MS). The detection limits (DLs) were range at 1.20 – 2.90 µg/mL. Histamine was detected in fish and fish products such as sardine (Sardinella gibosa) and mackerel (Scomberomorus guttatus) at concentration of 5.96 and 2.69 µg/mL, respectively, whereas cadaverine was found in sardine (Sardinella gibosa) at concentration of 4.96 µg/mL. Histamine...
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.
Foods
Monitoring of biogenic amines in food is important for quality control, in terms of freshness evaluation and even more for food safety. A novel and cost-effective method was developed and validated for the determination of the main biogenic amines: histamine, putrescine, cadaverine, spermidine and spermine in fish tissues. The method includes extraction of amines with perchloric acid, pre-column derivatization with Pyrene Sulfonyl Chloride (PSCl), extraction of derivatives with toluene, back-dissolution in ACN after evaporation and determination by reversed phase high performance liquid chromatography with UV and intramolecular excimer fluorescence detection. The structure of the pyrene-derivatives was confirmed by liquid chromatography–mass spectrometry with electrospray ionization. The standard addition technique was applied for the quantitation due to significant matrix effect, while the use of 1,7-diaminoheptane as internal standard offered an additional confirmation tool for th...
Determination of Biogenic Amines in_salmon and shrimp by CE_tandem MS.pdf.pdf
Biogenic amines are important indicators of freshness and quality in food. This application note presents the determination of 11 biogenic amines (spermine, spermidine, putrescine, histamine, cadaverine, agmatine, 2-phenyl-ethylamine, tyramine, tryptamine, urocanic acid, and serotonin) by capillary electrophoresis-tandem mass spectrometry (CE-MS/MS) in commercial samples of salmon and shrimp using a polyvinyl alcohol-coated (PVA) capillary, which increases the separation efficiency. The correlation coefficients of the calibration curves in the range of 0.02 to 100 µg/mL were greater than 0.998, and the limits of detection (LODs) and limits of quantification (LOQs) were in the range of 1.1-2.7 ng/mL and 3.6-8.9 ng/mL, respectively. Precision and accuracy were verified through recovery for spiked samples at three concentration levels (1, 2, and 5 mg/kg), in triplicate measurements. The recovery values ranged between 86 to 113% with RSD lower than 5.5%.
Journal of Chromatography A, 2005
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.
Determination of Biogenic Amines in Fish Products
Biogenic amines are nitrogenous organic bases produced during decarboxylation of amino acids or transamination of aldehydes and ketones in foods (1-3). The most important biogenic amines are histamine (HIS), tyramine (TYR), tryptamine (TRP), putrescine (PUT), and cadaverine (CAD), which are formed from the free amino acids histidine, tyrosine, tryptophane, ornithine, and lysine, respectively (1). High biogenic amine concentrations are randomly detected in fish and fish products, matured cheese, sausages, wine, and fermented vegetables like pickles. Formation of biogenic amines in aquatic products depends on different factors, such as the free amino acid contents in fish, the presence of bacterial biogenic amine decarboxylases, the quality parameters of raw materials, and environmental conditions (1). Many countries and international organizations have established regulations and legal requirements for maximum levels of biogenic amines (4). A histamine level lower than 50 mg/kg has been suggested by the U.S. Food and Drug Administration (FDA) as a guidance level in fish (5). The FDA has also recommended that 100 mg/kg of tyramine and 1,000 mg/kg of total biogenic amines should be tolerance levels in fish (5). In the European Union (EU), the acceptable level of histamine in Scombridae fish is suggested to be less than 100 mg/kg, and the maximum level of total biogenic amines should be less than 200 mg/kg in fish and fish products (6). According to Turkish
Monitoring the contents of biogenic amines in fish and fish products consumed in Korea
Food Control, 2010
In order to obtain the level of biogenic amines in fish and fish products, a reversed phase high performance liquid chromatographic method was used for the quantitation of 12 biogenic amines in 300 fish and 80 fish products in Korea. Biogenic amines were extracted with hydrochloric acid, derivatized with dansyl chloride, separated using gradient elution, and detected by photodiode array and all detected biogenic amines were identified by UPLC/MS/MS. The detection levels of biogenic amines in the sample ranged from ND (not detected
Journal of Food Measurement and Characterization, 2014
Biogenic amines forms in food by microbial enzymatic decarboxylation of amino acids and excessive consumption of these amines can be of health concern. Many techniques have been developed for the extraction of biogenic amines in food, including acidic or organic extraction as well as solid phase extraction. In this study, we described an alternative method based on a stirrer bead milling for extraction of biogenic amines from fish muscles. The rate and stirring time were optimized with an experimental design optimization procedure. The developed method was compared with the traditional homogenization extraction method. After a derivatization step with benzoyl chloride, samples were analyzed for amines quantitative determination with RP-HPLC system. The analysis method showed good linearity (correlation coefficients of 0.9989) and good recoveries ([94.23 %). The repeatability and reproducibility of the method, in terms of the relative standard deviation, ranged from 1.6 to 2.6 % and 3.3 to 4.9 % respectively. Moreover, the detection limits of biogenic amines were calculated between 0.05 and 0.09 mg kg-1 in fish samples. The proposed method has been applied to the analysis of different fish species of the Persian Gulf. Low biogenic amine levels were found in most fish samples. Total biogenic amine contents of selected samples were B68.3 mg kg-1 .