Method For Determination Of Histamine Research Articles

Stand out from matrix: Ultra-sensitive LC−MS/MS method for determination of histamine in complex biological samples using derivatization and solid phase extraction

The determination of low abundant endogenous components is a challenge for the clinical samples. Histamine, a crucial endogenous component, fulfils various regulatory and mediatory functions in human, and the change of content is a critical index for the diagnosis of some diseases, especially allergy, asthma, and anaphylactic shock. However, it is challenging to detect histamine because of the low stability and concentration in complex biological samples. Here we developed an ultra-sensitive and accurate LC−MS/MS quantification method based on derivatization, isotope dilution, and solid phase extraction. The derivatization of histamine with diisopropyl phosphite (DIPP) not only enhanced the retention on the LC column but also improved the ionization efficiency. Next, solid phase extraction was applied to remove the interference, which finally resulted in standing out of the trace histamine from the high contents of the matrix. The lowest limit of quantification (LLOQ) was 0.1 pg/mL that is enough low to determine the histamine in one cell and low nano-liter of serum. This approach was successfully applied for the quantification of histamine in clinical serum samples of asthma patients and mast cell treated with chemicals modulating histamine release.

Development and Validation of a TLC-Densitometry Method for Histamine Monitoring in Fish and Fishery Products.

Histamine poisoning is a significant public health problem. Therefore, the monitoring of histamine content in fish and fishery products is considered to be a crucial measure in the seafood industry. In the present study, a simple and rapid densitometric thin-layer chromatographic (TLC) method for histamine determination in fish samples was developed and validated. The samples were homogenized with 10% trichloroacetic acid and histamine was efficiently extracted. Then, an appropriate derivatization procedure was adopted with dansyl chloride. Once the derivatization was carried out, the samples were applied to silica gel TLC plates and developed by ascending chromatography with chloroform-triethylamine (6:4, v/v) as the mobile phase. The intensity of the histamine-dansyl derivative spots was measured by densitometry at 365 nm, and the quantitation was performed by BIO-1D image processing software. The validation of this method revealed good linearity and specificity over a concentration range from 6.25 to 100 mg/kg. Adequate precision was shown by relative standard deviations (RSD) smaller than 4.82%, accuracy ranged from −6.88% to 5.28%, and satisfactory recoveries ranging from 93% to 105% were obtained. The Limit of Detection and the Limit of Quantification were calculated at 4.4 mg/kg and 10.5 mg/kg, respectively. In addition, the effectiveness of the proposed method was assessed by the analysis of various samples, and the obtained results were confirmed with those achieved by the HPLC-UV method. Moreover, the developed method was found to be simple, cheap, and suitable for application to analyze several samples simultaneously.

Validation of HPLC Method for Determination of Histamine in Human Immunoglobulin Formulations.

Histamine fixed-immunoglobulin formulations, which consisted of 0.15 µg of histamine dihydrochloride and 12 mg of human immunoglobulin in a vial, are used for anti-allergic treatments, and controlling the amounts of histamine in the formulations is essential to avoid histamine intoxication. A high-performance liquid chromatography (HPLC) method for determination of histamine contents of the formulations was established and validated. Histamine extracted from the formulation was labeled with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate and was analyzed by gradient elution HPLC with UV detection at 260 nm. The method showed linearity in the range 0.8-2.4 µM (R > 0.999), accuracy (100.1-105.8% recovery), and precision (relative standard deviation ≤ 1.93%). The validated method was applied for five lots of the pharmaceutical, and their histamine contents were determined to be 0.149-0.155 µg/vial. These results indicated that the validated method is useful to control amounts of histamine in biopharmaceutical products. The HPLC method was developed for quantitative determination of histamine content of the histamine fixed-immunoglobulin formulations.

Determination of Histamine by a Rapid Fluorescamine-UPLC Method

We have developed a rapid analysis method for determination of histamine using ultra-performance liquid chromatography and fluorescamine derivatization. Histamine was extracted from foods with trichloroacetic acid after homogenization. The supernatant obtained by centrifugation was filtered and derivatized without solid-phase extraction. The mobile phase was 10 mM phosphate-acetonitrile (75 : 25) without ion-pairing. Recovery tests of histamine from fishes, seasoning and fish products gave acceptable recovery (95.8-117.7%). This method should be useful for rapid evaluation of food poisoning outbreaks.

Photoluminescence suppression effect caused by histamine on amino-functionalized graphene quantum dots with the mediation of Fe3 +, Cu2 +, Eu3 +: Application in the analysis of spoiled tuna fish

In this work, the photoluminescence of aqueous dispersion of amino-functionalized graphene quantum dots (GQDs-amino), with average size of 28nm, was studied in the presence of histamine when interaction was mediated by different metal ions. Stronger and selective interaction towards histamine occurred in the presence of Eu3+, Fe3+ and Cu2+. The sensibility of the normalized photoluminescence suppression curves (Ks) indicated a ten time stronger interaction of histamine with the surface of the GQDs in the presence of Fe3+. The linear response observed in the GQDs-amino-Fe3+ (luminescence at 345/435nm) covered the histamine concentration from 4.3×10−7molL−1 (limit of quantification) to 3.2×10−5molL−1. The GQDs-amino-Fe3+ was applied as a probe in the analysis of tuna fish samples after cationic solid phase extraction. Analytical results were statistically similar to the ones achieved with a reference HPLC-fluorescence (after chemical derivatization) based method. The proposed method for determination of histamine is simple, does not involve the use of toxic labeling reagents and can easily be adapted for routine quality control analysis of fish and related foodstuffs.

A Novel Spectrophotometric Method for Determination of Histamine Based on Its Complex Reaction with Ni(II) and Alizarin Red S

The development of analytical methods of histamine using Ni (II) and alizarin red S reagents by UV-Vis spectrophotometry has been done. The objective of this research is to determine the ability of Ni(II) and alizarin red S to form color complex compound with histamine and it will be used to detect the presence of histamine qualitatively and quantitatively as well. Absorbance was measured at a maximum wavelength of 604 nm. In this method, it has been carried out optimization of analytical parameters such as the concentration of Ni(II), the concentration of alizarin red S, pH, and respond time. Analytical parameter optimization showed concentration of Ni(II) is 20 ppm, alizarin red S 75 ppm, pH 8, and a respond time of 15 minutes. Method validation indicated that the coefficient of variation, detection limit, and the limit of quantitation are 0.245%; 9.49 ppm; and 31.62 ppm respectively with a sensitivity of 0.0063/ppm and linearity of 0.99. Accuracy to histamine with a concentration of 50, 75, and 125 ppm are 105.87%, 101.06%, 97.21%, respectively.

A Novel Method for Determination of Histamine in Tuna Fish by Ion Mobility Spectrometry

Ion mobility spectrometry (IMS) was used for determination of the histamine content in samples of tuna stomach, and the results were compared with measurements by high-pressure liquid chromatography (HPLC) that is considered the “gold standard” method. The production of histamine as a function of storage time at ambient temperature (25–29 °C) was followed by both methods and a good correlation was found between them. The results were validated by IMS and HPLC measurements of samples of fresh tuna fillets in which the initial histamine level was below 10 mg histamine per kg (10 ppm). The level gradually increased to thousands of milligrams per kilogram after about 30 h at ambient temperature. In the IMS measurements, the intensity ratio between the fragment ion of histamine (K0 = 2.73 cm2 V−1 s−1) and the sum of all the ions in the mobility spectrum served to quantify the histamine level in the fish samples. Thus, a rapid, simple, and inexpensive method was developed for determination of histamine in tuna.

Optimization and Validation of Analytical Method for Determination of Histamine in Fish using HPLC-FLD

Optimization and Validation of Analytical Method for Determination of Histamine in Fish using HPLC-FLD

Determination of Histamine in Wine Samples by Flow-Injection Analysis and Multivariate Calibration

A flow injection method for the rapid determination of histamine in wines is proposed. This method is based on the reaction of the analyte with 1,2-naphthoquinone-4-sulfonate to form a derivative detected by UV-Vis absorption spectroscopy. The amine derivatization is carried out at pH 9.2 in a PTFE coil heated at 60°C. Experimental conditions are not able to provide selectivity for histamine with respect to other amino compounds so that its response is interfered with by other amines and amino acids present in the wine matrix. Here, multivariate calibration methods have been used to overcome the lack of selectivity. As a result, wines can be directly analyzed without removing interferences. For this purpose, spectra taken at the peak maximum have been used as multivariate data to be further analyzed with partial least square regression. The number of significant latent variables to be used in the construction of the calibration models as well as a preliminary evaluation of the prediction performance have been estimated by leave-one-out cross validation. The quantification of histamine concentrations in wine samples is satisfactory with an overall prediction error about 5%.

Ultrasensitive flow-injection electrochemical method for determination of histamine in tuna fish samples

Histamine is a potentially hazardous compound and one of the major concerns in food chemistry. High amount of histamine may be found in food as a consequence of the use of poor quality raw materials, contamination and inappropriate conditions during food processing and storage. A novel method for the determination of histamine in flow-injection systems has been developed for use in seafood quality inspection and food quality control laboratories. The developed technique is very simple, precise, accurate, time saving and economic as compared to all of the previously reported methods. The effects of various parameters on the sensitivity of the method were investigated. The best performance was obtained with the conditions, pH value of 2.0, and sweep rate value of 40 V/s, accumulation potential of 900 mV and accumulation time of 0.4 s. In this work, we introduce a special computer based numerical method, for calculation of the analyte signal and noise reduction. The electrode response was calculated based on partial and total charge exchanges at the electrode surface after subtracting the background current from noise. The waveform potential consisting of potential steps for cleaning and accumulation of analyte, and potential ramp was applied on an Au disk microelectrode (with a radius of 12.5 μm). The method was linear over the concentration range of 1.1–5555 pg/ml (r = 0.998) with a limit of detection and quantification 0.35 and 1.16 pg/ml, respectively.

Determination of Histamine in Rat Plasma and Tissue Extracts by Intramolecular Excimer-Forming Derivatization and LC with Fluorescence Detection

A highly sensitive and selective method for determination of histamine in rat plasma and tissue extracts by liquid chromatography with fluorescence detection is described. The method is based on precolumn derivatization of amino groups of histamine with two molecules of 4-(1-pyrene)butyric acid N-hydroxysuccinimide ester that allows generation of intramolecular excimer fluorescence. The detection limit for histamine was 0.183 nM. This sensitivity allowed determination of histamine in 10 μL of rat plasma or in the extracts from less than 1 mg of tissue.

A rapid determination of histamine and 3-methylhistamine in human plasma by high performance liquid chromatography

Histamine plays an important pathophysiological role in allergy, inflammation, gastric acid secretion, microcirculation and neurotransmission. 3-Methylhistamine is a prominent metabolite of histamine. Different methods for determination of histamine in biological fluids have been developed. In the present study, a simple, simultaneous determination of histamine and 3-methylhistamine by HPLC (precolumn derivatization with fluorescamine) was developed in human plasma using fluorescence detection with 1-methylhistamine as the internal standard. Linear regression analysis of the ratios of the concentrations of histamine and 3-methylhistamine (X) against peak height ratios (Y) yielded the following: y = 0.0073x − 0.0096 (R 2 = 0.990) and y = 0.0077x − 0.0111 (R 2 = 0.989). In conclusion, it was possible to detect histamine and 3-methylhistamine below 5 ng mL−1 in 1 mL plasma.

Improved enzymatic method for the rapid determination of histamine in wine

Fermented foods are frequently contaminated by histamine generated by microorganisms possessing histidine decarboxylase activity. The ingestion of large amounts of histamine can cause serious toxicological problems in man. Thus, it becomes important to set a reliable method for rapid histamine quantification in foods. The detection of bacteria exhibiting histidine decarboxylase activity is also important to estimate the risk of contamination of food. Previous enzymatic methods used to quantify histamine in fish gave erroneously high values due to interference when applied to wine. A new enzymatic method is described that allows the direct determination of histamine concentrations in this type of sample. It can be used for the detection of histamine in synthetic media, grape must or wine (white, rosé, red) without polyphenols or sugar interferences. This new enzymatic method shows a good correlation (R 2 = 0.996, p<0.001) between the histamine concentrations and absorbances in the interval 0.4–160 mg l−1. Comparison between this enzymatic method and a high-performance liquid chromatography method showed a high correlation (R 2 = 0.9987, p<0.001). A miniaturized enzymatic method is also proposed, which is particularly useful when high numbers of samples must be analysed.

A simple and rapid method for colorimetric determination of histamine in fish flesh

Histamine is a significant chemical hazard in fish. It is derived from the bacterial decarboxylation of amino acid histidine, that is present in large amounts in fish of Scombridae family and its presence is considered as a good indicator of temperature abuse and the state of good manufacturing practices adopted in the handling of such fish. A simple and rapid chemical method for determination of histamine in fish flesh is reported for use in seafood quality inspection laboratories. Good recoveries (>91%) were obtained for histamine at spiking levels ranging 1–60 mg/100 g. The overall precision (relative standard deviation, %) in the new assay ranged from 2.61 to 9.63. The interaction between the imidazole ring and p-phenyldiazonium sulfonate was made the basis of a quantitative colorimetric method for estimation of histamine. The results of the new assay showed a high correlation ( R 2=0.999) with the assay of Hardy and Smith [J. Sci. Food Agric. 27 (1976) 595] in the recovery of histamine. The limit of detection was 1 mg/100 g for the new assay and was comparable with the existing methods. A concentration-based reference color scale is provided for the determination of defect and hazard action levels set by the regulatory agencies. Visual comparison of color intensity of test samples with standard concentrations in reference color scale for determining these levels without the aid of a spectrophotometer was an important practical application for rapidly estimating histamine in fresh fish fulfilling one of the HACCP requirements. The assay was simple requiring no laborious treatments, and may be suitable for routine analysis in monitoring of histamine in fish.

Rapid Method for Biogenic Amines Evaluation in Fish Meal

A novel enzyme-based colorimetric method for hista-mine determination in fish meal was developed. It is based upon hista-mine oxidation by diamine oxidase and detection of the hydrogen peroxide generated using a peroxidase catalyzed reaction coupled with phenol-aminoantipyrine. At optimum assay conditions (temperature: 50°C, pH: 9.0), this technique allowed the accurate quantification of histamine + putrescine + cadaverine levels (amine index) between 200 to 2000 ppm. The method represents a good alternative for the rapid detection of potentially toxic fish meal.

Determination of histamine in fish products by capillary electrophoresis and ion-pair liquid chromatography with diode-array detection

A method for histamine determination in fish and fish products by capillary electrophoresis and ion-pair liquid chromatography has been developed. Histamine was extracted from different fish samples with 10% trichloroacetic acid, and the filtrate was directly applied to capillary electrophoresis apparatus. A preliminary purification through a solid phases extraction cartridge (Sep-pak C18) was necessary for HPLC analysis. Histamine was detected ‘on-line’ at 210 nm by both approaches. HPLC procedure allowed accurate (±2.2%) and repeatable (±1.6%) determination of histamine in fish products at appropriate levels (20–100 mg kg−1) to meet current regulations. © 1999 Society of Chemical Industry

P-433 - A New Luminescent Detection Method for Determination of Histamine and N^-Methyl- histamine Using HPLC Coupled with Immobilization Diamine Oxidase.

P-433 - A New Luminescent Detection Method for Determination of Histamine and N^-Methyl- histamine Using HPLC Coupled with Immobilization Diamine Oxidase.

An improved automated fluorimetric method for determination of histamine

The automated continuous flow system for the extraction and fluorimetric analysis of histamine based on the principle of Shore et al. (1959) has been improved. With lower consumption of reagents and further simplification of the working conditions, histamine can be determined quantitatively in a routine fashion in aqueous samples, with or without protein content, up to a concentration of approximately 0.1 ng/ml. The rate of analysis is 30 samples/h.

Simple and Rapid Paper Chromatographic Method for the Simultaneous Determination of Histidine and Histamine in Fish Samples

A simple and rapid method for the simultaneous determination of histamine and histidine in fish samples is described. The method entails paper chromatography and is sensitive from 0.5 mug to at least 30 mug. The method is reproducible to within +/- 5% and compares favorably with a biological method for histamine determination.

Formation and Binding of Histamine by Free Mast Cells of Rat Peritoneal Fluid

Suspensions of the cells of rat peritoneal fluid have a marked ability to decarboxylate C14 l-histidine and bind the resulting histamine in stable form. The evidence is strong that this activity is due almost entirely to mast cells; these constitute about 4% of the total number of cells present. The effects of temperature, time, and ph on this process were found to be characteristic of enzymic reactions. Preincubation of cell suspensions with nonisotopic histamine had no effect on the formation and binding of C14 histamine; this is evidence that exogenous histamine cannot enter the bound condition in free mast cells. The effects of histidine analogs on binding is described. Disruption of the mast cells results in a considerable loss in histamine forming activity. However, a fairly stable, soluble histidine decarboxylase can be obtained from the disrupted cells. A new method for determination of histamine as the S35 dibenzenesulfonyl derivative is described.