{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,10,7]],"date-time":"2026-10-07T19:29:32Z","timestamp":1791401372102,"version":"4.3.3"},"reference-count":38,"publisher":"MDPI AG","issue":"16","license":[{"start":{"date-parts":[[2020,8,8]],"date-time":"2020-08-08T00:00:00Z","timestamp":1596844800000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Molecules"],"abstract":"<jats:p>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 \u22126.88% 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.<\/jats:p>","DOI":"10.3390\/molecules25163611","type":"journal-article","created":{"date-parts":[[2020,8,10]],"date-time":"2020-08-10T09:04:16Z","timestamp":1597050256000},"page":"3611","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":23,"title":["Development and Validation of a TLC-Densitometry Method for Histamine Monitoring in Fish and Fishery Products"],"prefix":"10.3390","volume":"25","author":[{"given":"Ayoub","family":"Kounnoun","sequence":"first","affiliation":[{"name":"Laboratory of Applied Biology and Pathology, Department of Biology, Faculty of Sciences of Tetouan, Abd Al Malek Essaadi University, Tetouan 93000, Morocco"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Adnane","family":"Louajri","sequence":"additional","affiliation":[{"name":"Laboratory of Applied Biology and Pathology, Department of Biology, Faculty of Sciences of Tetouan, Abd Al Malek Essaadi University, Tetouan 93000, Morocco"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1296-7633","authenticated-orcid":false,"given":"Francesco","family":"Cacciola","sequence":"additional","affiliation":[{"name":"Department of Biomedical, Dental, Morphological and Functional Imaging Sciences, University of Messina, 98125 Messina, Italy"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hafssa","family":"El Cadi","sequence":"additional","affiliation":[{"name":"Laboratory of Valorization of Resources and Chemical Engineering, Department of Chemistry, Abdelmalek Essa\u00e2di University, Tangier 90000, Morocco"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hajar","family":"Bougtaib","sequence":"additional","affiliation":[{"name":"Laboratory of Applied Biology and Pathology, Department of Biology, Faculty of Sciences of Tetouan, Abd Al Malek Essaadi University, Tetouan 93000, Morocco"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Naoual","family":"Alahlah","sequence":"additional","affiliation":[{"name":"Regional Analysis and Research Laboratory, National Office of Food Safety ONSSA, Tangier 90000, Morocco"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1366-1612","authenticated-orcid":false,"given":"Aicha","family":"El Baaboua","sequence":"additional","affiliation":[{"name":"Laboratory of Applied Biology and Pathology, Department of Biology, Faculty of Sciences of Tetouan, Abd Al Malek Essaadi University, Tetouan 93000, Morocco"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8646-2043","authenticated-orcid":false,"given":"Mohamed","family":"El Maadoudi","sequence":"additional","affiliation":[{"name":"Regional Analysis and Research Laboratory, National Office of Food Safety ONSSA, Tangier 90000, Morocco"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2020,8,8]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"343","DOI":"10.1016\/j.envres.2008.12.002","article-title":"Perceptions of the risks and benefits of fish consumption: Individual choices to reduce risk and increase health benefits","volume":"109","author":"Burger","year":"2009","journal-title":"Environ. Res."},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"1547","DOI":"10.1080\/19440049.2011.600728","article-title":"Biogenic amines in fish, fish products and shellfish: A review","volume":"28","author":"Prester","year":"2011","journal-title":"Food Addit. Contam. Part A"},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1016\/j.ab.2012.09.022","article-title":"Simultaneous electrochemical measurement method of histamine and N\u03c4-methylhistamine by high-performance liquid chromatography\u2013amperometry with o-phthalaldehyde\u2013sodium sulfite derivatization","volume":"432","author":"Maldonado","year":"2013","journal-title":"Anal. Biochem."},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"181","DOI":"10.1016\/j.foodcont.2016.12.001","article-title":"A rapid screening of histamine concentration in fish fillet by direct analysis in real time mass spectrometry (DART-MS)","volume":"75","author":"Nei","year":"2017","journal-title":"Food Control"},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1155\/2014\/482531","article-title":"Histamine poisoning from ingestion of fish or scombroid syndrome","volume":"2014","author":"Tortorella","year":"2014","journal-title":"Case Rep. Emerg. Med."},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"1131","DOI":"10.1080\/10408398.2016.1242476","article-title":"Histamine food poisonings: A systematic review and meta-analysis","volume":"58","author":"Colombo","year":"2018","journal-title":"Crit. Rev. Food Sci. Nutr."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"1013","DOI":"10.1016\/j.foodcont.2008.12.001","article-title":"Isolation and identification of histamine-forming bacteria in tuna sandwiches","volume":"20","author":"Kung","year":"2009","journal-title":"Food Control"},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"15","DOI":"10.1556\/JPC.22.2009.1.3","article-title":"Densitometric TLC analysis of histamine in fish and fishery products","volume":"22","author":"Bajc","year":"2009","journal-title":"JPC J. Planar Chromatogr."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"893","DOI":"10.1007\/s10337-020-03909-9","article-title":"Development and Validation of a High-Performance Liquid Chromatography Method for the Determination of Histamine in Fish Samples Using Fluorescence Detection with Pre-column Derivatization","volume":"83","author":"Kounnoun","year":"2020","journal-title":"Chromatographia"},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"756","DOI":"10.1016\/j.foodchem.2010.11.060","article-title":"Development and validation of an HPLC-FLD method for rapid determination of histamine in skipjack tuna fish (Katsuwonus pelamis)","volume":"126","author":"Tahmouzi","year":"2011","journal-title":"Food Chem."},{"key":"#cr-split#-ref_11.1","unstructured":"EC (2005). Commission Regulation"},{"key":"#cr-split#-ref_11.2","unstructured":"(EC) No 2073\/2005 of 15 Novembre 2005 on the microbiological criteria for foodstuffs. Off. J. Eur. Comm., 338, 1-26."},{"key":"ref_12","unstructured":"EU, European Union (2014). Report EUR 26605 EN. Equivalence Testing of Histamine Methods\u2014Final Report, Joint Research Centre. Administrative Arrangement NL SANCO\/2011\/G4\/JRC32515\/."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"70","DOI":"10.1016\/j.chroma.2008.09.028","article-title":"Development of an automated on-line pre-column derivatization procedure for sensitive determination of histamine in food with high-performance liquid chromatography\u2013fluorescence detection","volume":"1209","author":"Peng","year":"2008","journal-title":"J. Chromatogr. A"},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"329","DOI":"10.1016\/S0308-8146(03)00005-0","article-title":"A rapid gas chromatographic method for the determination of histamine in fish and fish products","volume":"82","author":"Hwang","year":"2003","journal-title":"Food Chem."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"1475","DOI":"10.1016\/j.foodchem.2006.08.028","article-title":"A review: Current analytical methods for the determination of biogenic amines in foods","volume":"103","year":"2007","journal-title":"Food Chem."},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"399","DOI":"10.1016\/j.lwt.2010.08.011","article-title":"Use of small diameter column particles to enhance HPLC determination of histamine and other biogenic amines in seafood","volume":"44","author":"Dalgaard","year":"2011","journal-title":"LWT Food Sci. Technol."},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"465","DOI":"10.1016\/j.foodcont.2004.05.008","article-title":"A simple and rapid method for colorimetric determination of histamine in fish flesh","volume":"16","author":"Patange","year":"2005","journal-title":"Food Control"},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"255","DOI":"10.1016\/S0308-8146(01)00173-X","article-title":"A comparison of the TLC-densitometry and HPLC method for the determination of biogenic amines in fish and fishery products","volume":"75","author":"Shakila","year":"2001","journal-title":"Food Chem."},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"129","DOI":"10.1016\/S0021-9673(99)01132-2","article-title":"Thin-layer chromatography in food and agricultural analysis","volume":"880","author":"Sherma","year":"2000","journal-title":"J. Chromatogr. A"},{"key":"ref_20","unstructured":"AOAC (2005). Association of Official Analytical Chemists. Histamine in Seafood, Fluorimetric Method 977.13. AOAC Off Method, AOAC."},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"1154","DOI":"10.1016\/j.foodcont.2010.12.014","article-title":"A simple and rapid method for histamine analysis in fish and fishery products by TLC determination","volume":"22","author":"Tao","year":"2011","journal-title":"Food Control"},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"547","DOI":"10.1016\/j.foodchem.2017.03.081","article-title":"Tuneable surface enhanced Raman spectroscopy hyphenated to chemically derivatized thin-layer chromatography plates for screening histamine in fish","volume":"230","author":"Xie","year":"2017","journal-title":"Food Chem."},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"3386","DOI":"10.1039\/C8AY00336J","article-title":"Rapid determination of histamine in fish by thin-layer chromatography-image analysis method using diazotized visualization reagent prepared with p-nitroaniline","volume":"10","author":"Yu","year":"2018","journal-title":"Anal. Meth."},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"1392","DOI":"10.1016\/j.foodchem.2012.06.022","article-title":"Determination of biogenic amines in wine by thin-layer chromatography\/densitometry","volume":"135","author":"Romano","year":"2012","journal-title":"Food Chem."},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"4226","DOI":"10.1016\/j.foodchem.2013.06.005","article-title":"The use of aqueous normal phase chromatography as an analytical tool for food analysis: Determination of histamine as a model system","volume":"141","author":"Dang","year":"2013","journal-title":"Food Chem."},{"key":"ref_26","doi-asserted-by":"crossref","first-page":"2425","DOI":"10.1080\/10826070600864908","article-title":"Application of the Iodine-Azide Procedure for Detection of Biogenic Amines in TLC","volume":"29","author":"Ciesielski","year":"2006","journal-title":"J. Liq. Chrom. Relat. Technol."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"281","DOI":"10.1007\/s11694-016-9395-z","article-title":"Histamine levels in Indian fish via enzymatic, TLC and HPLC methods during storage","volume":"11","author":"Arulkumar","year":"2017","journal-title":"J. Food Meas. Charact."},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"223","DOI":"10.1016\/j.chroma.2004.06.014","article-title":"New solvent systems for thin-layer chromatographic determination of nine biogenic amines in fish and squid","volume":"1045","author":"Pickova","year":"2004","journal-title":"J. Chromatogr. A"},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"117","DOI":"10.1016\/S0308-8146(98)00113-7","article-title":"Simple, rapid and valid thin layer chromatographic method for determining biogenic amines in foods","volume":"65","author":"Shalaby","year":"1999","journal-title":"Food Chem."},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"767","DOI":"10.1007\/s10337-020-03896-x","article-title":"Dansyl Chloride as a Derivatizing Agent for the Analysis of Biogenic Amines by CZE-UV","volume":"83","author":"Mantoanelli","year":"2020","journal-title":"Chromatographia"},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"1097","DOI":"10.1093\/jaoac\/82.5.1097","article-title":"Relevance of matrix effect in determination of biogenic amines in plaice (Pleuronectes platessa) and whiting (Merlangus merlangus)","volume":"82","author":"Duflos","year":"1999","journal-title":"J. AOAC Int."},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"97","DOI":"10.1016\/j.ijfoodmicro.2018.07.023","article-title":"Validation of standard method EN ISO 19343 for the detection and quantification of histamine in fish and fishery products using high-performance liquid chromatography","volume":"288","author":"Duflos","year":"2019","journal-title":"Int. J. Food Microbiol."},{"key":"ref_33","doi-asserted-by":"crossref","first-page":"694","DOI":"10.1016\/j.foodchem.2016.05.111","article-title":"European official control of food: Determination of histamine in fish products by a HPLC\u2013UV-DAD method","volume":"211","author":"Altieri","year":"2016","journal-title":"Food Chem."},{"key":"ref_34","doi-asserted-by":"crossref","first-page":"4128","DOI":"10.1016\/j.chroma.2009.02.045","article-title":"Thin-layer chromatography for the identification and semi-quantification of biogenic amines produced by bacteria","volume":"1216","year":"2009","journal-title":"J. Chromatogr. A"},{"key":"ref_35","unstructured":"Directive EC Council (2002). 657\/EC of 12 August, 1990 on implementing Council Directive 96\/23\/EC concerning the performance of analytical methods and the interpretation of results. J. Eur. Communit., 221, 8\u201336."},{"key":"ref_36","unstructured":"Afnor French Standardization Association (2010). Analysis of Agri-Foodstuffs\u2014Protocol of Characterization for the Validation of a Quantitative Method of Analysis by Construction of an Accuracy Profile, Afnor. NF F03-110."},{"key":"ref_37","unstructured":"ISO International Organization for Standardization (2017). Microbiology of the Food Chain-Detection and Quantification of Histamine in Fish and Fishery Products, ISO. ISO 19343."}],"container-title":["Molecules"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1420-3049\/25\/16\/3611\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,11]],"date-time":"2025-10-11T09:58:15Z","timestamp":1760176695000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1420-3049\/25\/16\/3611"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2020,8,8]]},"references-count":38,"journal-issue":{"issue":"16","published-online":{"date-parts":[[2020,8]]}},"alternative-id":["molecules25163611"],"URL":"https:\/\/doi.org\/10.3390\/molecules25163611","relation":{},"ISSN":["1420-3049"],"issn-type":[{"value":"1420-3049","type":"electronic"}],"subject":[],"published":{"date-parts":[[2020,8,8]]}}}