Quality control of the analysis of histamine in fish by proficiency test (original) (raw)

Quality assurance of histamine analysis in fresh and canned fish

Food Chemistry, 2016

Histamine determination is relevant for fish safety, quality and trade. Recently a study by the European Union (EU) compared the Codex and the EU mandated methods for the analysis of histamine and observed that they underestimated and overestimated the results, respectively. To solve this problem, a simple and efficient procedure for the extraction and quantification of histamine by ion-pair HPLC method with post-column derivatization and fluorimetric detection is proposed. It was optimized and validated for the analysis of histamine in fish. The method attended the performance criteria established by Commission Decision 2002/657/CE. The method was also submitted to proficiency testing; uncertainty was calculated; and the stability of solutions and standards was investigated. There was no matrix effect. The LOD, LOQ, CCa and CCb were fit for the purpose. The method was successfully used in the analyses of freshwater fish and fresh and canned tuna.

High-throughput histamine analysis approach in an official control laboratory: Analytical methods and four years fish products results

2014

A highly practical two-tier approach involving a screening and a confirmatory method was set up to efficiently test histamine in fish products in the frame of official controls. After their validation, the routine management of the two procedures was simplified as far as possible ensuring a strict quality data control and maximizing the cost-effectiveness. Accordingly five hundred and ninety batches of fish products (3129 determinations) sampled from the Italian authorities were successfully analyzed over a four year period (2008-2012). Only a small percentage of analysed batches (4.9%) was judged non-compliant. The examination of irregular cases (fish species, processing technology and storage practices) suggests important considerations in order to minimise the histamine risk for consumers.

A simple and rapid method for histamine analysis in fish and fishery products by TLC determination

A simple and rapid thin-layer chromatography (TLC)-densitometry method for histamine analysis in fish and fishery products was established. Histamine was extracted from seafood with 80% ethanol. The sample extracts and standard solutions of histamine were applied to cellulose TLC plate and developed by ascending chromatography with ammoniaeethanol 1:3 (v/v) as mobile phase. Histamine was visualized with pauly's reagent, the intensity of the colored spots was digitized and calculated by image processing method software, Lane & Spot Analyzer (ATTO, Tokyo, Japan). Successful separation of histamine from other (imidazole compounds) pauly's reagent-positive components in 80% ethanol fish extracts was achieved. The linearity of the histamine estimation using this method was good within the range from 30 ng to 1000 ng of histamine (r 2 ¼ 0.9997). Histamine can be satisfactorily detected and completely separated from histidine, 4-methyl-imidazole and other pauly's reagent-positive compounds. This method does not need expensive instrument, any tedious pretreatment to eliminate potential interference other imidazole compounds such as histidine or carnosine. It is also less reagents compared with HPLC method. Moreover, it is a simple, rapid, sensitive, reproducible. Therefore this method is suitable for monitor of histamine in multiple fish and fishery products simultaneously that contain as little as 20 ppm histamine (2.0 mg/100 g).

Determination of Histamine in Various Marine Fish Species Available in Major Markets of Punjab, Pakistan by LC-MS/MS

2018

Fish samples from selected five (5) major markets of Punjab (Lahore, Faisalabad, Multan, Rawalpindi and Gujranwala) were collected randomly consisting of nine (9) marine fish species. LCQ Fleet with ion trap mass analyzer coupled with Surveyorplus pump and Surveyorplus degassor of Thermoscientific was used for histamine determination in present study. The histamine detected in different nine (9) samples from different markets was within safe limits. The fishes were also examined for appearance, texture, odour and presence of black spots. All the physical parameters were within normal range. It was concluded that the marine fish species being sold in various fish markets of Punjab province are fresh with good physical conditions and having histamine in safe limits.

Commercial test kits and the determination of histamine in traditional (ethnic) fish products-evaluation against an EU accepted HPLC method

Food Chemistry, 2011

Although commercial test kits are generally used and/or evaluated for determining histamine in fresh and canned fish, and fish meal, there is little information on their performance and the application for traditional fish products (TFPs), which generally differ in product properties. In this study, three quantitative (Food EIA, Veratox, Histaquant) and four qualitative (Histasure, Histameter, Transia qualitative and semiquantitative) commercial histamine test kits were evaluated against HPLC method for detecting histamine in several traditional fish products. Among the quantitative kits, Histamine Food EIA showed the best correlation with HPLC method for TFPs (R 2 = 0.9132) as well as good recoveries ranging between 89 (±4.11)% and 117 (±1.50)%. Although good recoveries were also observed with Veratox kit, poor correlation was found with HPLC. Poor correlation and low recoveries were also observed with Histaquant. Histasure and Transia tube histamine kits showed good agreement with HPLC results. However, the detection limit for Transia qualitative kit is 100 ppm, and for Histasure and Transia semi-quantitative kits can be set to 50 ppm. Therefore, Histasure and Transia semi-quantitative kits are found more suitable for either HACCP monitoring histamine in seafood processing plants or regulatory purposes according to Food Drug and Administration (FDA) legislation for TFPs. However, Transia semi-quantitative kit should be used in caution for histamine cut off values <50 ppm. This study shows that each test kit can represent different performance for determining histamine in TFPs according to product type, and therefore new commercial test kits should be evaluated against an approved analytical method before applications in future for these types of products.

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

2015

Article history: Received 01 July 2015 Accepted 29 July 2015 In the present study, simple and reliable method of histamine analysis was developed, optimized and validated to meet the requirements of fish safety. Histamine in fish samples was extracted with a methanol–phosphate buffer including 2 % TCA solution (50:50, v/v) followed by defatting with hexane after centrifugation at 13,000 rpm. Histamine was separated, identified by reversed phase high performance liquid chromatography (HPLC) with gradient mobile phase (methanol–phosphate buffer at pH 3.5) and quantified by fluorescence detector at excitation: 345 nm, emission: 445 nm after on-line derivatization with O-phathalaldehyde in a pre-column derivatization step using automatic injection program. The method was validated with average recovery 96% and coefficient of variation (CV %) less than 8 %. The uncertainty was estimated and was set to ±26.4 %. The performance of the proposed method was checked with a sample from the Food...

Determination of histamine levels by LC-MS/MS in various fish species available in the local markets of Punjab, Pakistan

2016

Sixty apparently fresh and properly iced samples of fish species were randomly collected from five major markets of Punjab, Pakistan. These samples were transported to the Fish Quality Control Laboratory, FR&TI, Lahore kept in ice boxes and temperatures below -1 oC. The samples were examined for Physical Parameters including Appearance, Glazing, Texture, Odour, Presence of Black Spots and Chemical Parameter including determination of Histamine levels by LCMS/MS. All Physico-Chemical Parameters were found within normal range. Histamine was either not detected or found within permissible limits as compared with International Standards for human consumption. In conclusion, significant decomposition and histamine formation can be avoided by good fish handling practices including icing or rapid immersion of the catch in chilled water followed by uninterrupted frozen storage.

UPLC-MS/MS determination of histamine levels in canned fish collected from Belgrade retail markets

2016

The aim of this study was to determine the amount of histamine in canned fish samples collected from Belgrade retail stores using ultra-performance liquid chromatography tandem mass-spectrometry. In addition, the established levels were compared with the maximum levels set by US Food and Drug Administration (FDA) and European Union (EU) in order to assess the risk of this toxic biogenic amine to the city population. Histamine was detected in 54.07% of analyzed canned fish, in concentrations ranging from 5 to 420 mg/kg with a mean level of 60.91 mg/kg. In canned tuna, histamine levels ranged from 6 to 420 mg/kg, while in canned mackerel the concentrations ranged from 5 to 121 mg/kg. Also, the mean histamine level in canned tuna was higher than in canned mackerel (mean values were 60.91 mg/kg and 42.94 mg/kg, respectively). Among the tested canned fish, 20% of samples had higher histamine levels than the maximum level prescribed by the FDA (histamine levels >50 mg/kg), indicating d...

Validation of standard method EN ISO 19343 for the detection and quantification of histamine in fish and fishery products using high-performance liquid chromatography

International Journal of Food Microbiology, 2019

In contaminated fish, bacterial decarboxylases produce histamine from histidine, thereby causing scombroid fish poisoning. European Regulation (EC) No 2073/2005 on microbiological criteria for foodstuffs requires using a fully validated, standardized reference HPLC method for detecting and quantifying histamine. After optimizing this reference method for the quantification of histamine in fish muscle, we organized an inter-laboratory study in 2013 across nine laboratories from seven European countries using defined criteria of method performance. The optimized, validated method was standardized (Standard EN ISO19343) as part of Mandate M381 from the European Commission to the European Committee for Standardization (CEN), signed in December 2010. The standard method was validated for three types of foodstuffs (fish with enzymatic maturation, fish without enzymatic maturation and fish sauce).

Histamine levels in Indian fish via enzymatic, TLC and HPLC methods during storage

Histamine is a potentially hazardous compound and one of themajor concerns in food chemistry. In the present study the histamine levels of 20 muscle sample for each milk fish (Chanos chanos) and Indianwhiting (Sillago indica) were analyzed with 6, 12, 18 and 24 h intervals and compared by enzymatic assay (EA), thin layer chromatography (TLC) and high performance liquid chromatography (HPLC) methods. During storage, histamine levels were ranged between 16.50 ± 1.63 and 48.13 ± 1.24 mg/100 g with a linear regression r2 = 0.855; P\0.05 for the milk fish as determined by the EA method.Whereas, histamine levels in Indian whiting was 19.86 ± 1.64–43.84 ± 2.44 mg/100 g with a linear regression r2 = 0.997; P\0.01. In the TLC method, histamine were observed at lower levels compared to the EA and HPLC and showing 4.77 ± 0.13–7.72 ± 0.16 and 6.81 ± 0.11–7.53 ± 0.15 mg/100 g in milk fish and Indian whiting muscle, respectively. The linear regression r2 = 0.835; P\0.05 was noted in both fishes. The HPLC analysis also confirmed that the histamine levels were ranged from 18.18 ± 1.03 to 28.69 ± 1.14 mg/100 g in milk fish with a linear regression r2 = 0.903; P\0.01. For Indian whiting fish, histamine was ranged from 17.28 ± 1.67 to 23.97 ± 1.27 mg/100 g with a linear regression r2 = 0.910; P\0.01. Therefore,monitoring of histamine is a critical task in the seafood industry. Our result showed that the TLC methods can be used to monitor the histamine content in routine analysis and enzymatic analysis can be used to quantify the levels of histamine in the seafood industry.