Optimization of The Performance of The Methodologies for Detection of Some Contaminants in Food
Abstract
This study provided to establish validated, accredited, a sensitive analytical methods for some compounds and metals expected to be contaminated fish and fish products. This should help various Egyptian fish products to penetrate international markets not only to enhance the international trade but also for consumer health impact. The applicability of the developed methods will be applied, as part of the national monitoring program for histamine, veterinary drug residues and heavy metals in Egyptian fish and fish products.
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 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 derivatisation 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%.
A list of 20 drugs from different classes including, sulfonamides, tetracyclines, macrolides, β- Lactam , quinolones and illegal antibiotics such as chloramphenicol was selected that are reported in European Commission Directives 3770/90/EEC and which is listed in annex IV in Council Directive 23/96/EC. The optimization parameters were studied to obtain the proper conditions of the instrument in terms of best sensitivity with lowest interference. The method performance characteristics is tested based on Commission Decision 2002/657/EC by measuring linearity, accuracy, repeatability, within-laboratory reproducibility, decision limit (CCα) and detection capability (CCβ) using LC-MSMS with electrospray ionization. Limit of quantification was 25 ug/kg for all drugs and 0.1 ug/kg for chloramphenicol with accepted mean recoveries ranged from 77-91 and CV% less than 13.
Also, heavy metals were studied as a source of fish contamination. An easy and optimized method was developed using atomic absorption spectrometer after microwave digestion for determination of 11 element including Pb, Cd, Cu, As, Hg, Zn, Fe, Al, Cr, Mn and Sn. Mean recoveries ranged between 81-117% and CV% was less than 1 for all metals.
The methods performance was extra tested using external proficiency tests to evaluate the compliance with │Z│ score; which showed satisfactory results. The methods were accredited by the Finnish Accreditation Service body (FINAS) according to ISO/IEC 17025.
Thirty four fish samples were subjected to histamine assessment using the validated
Abstract
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 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 derivatisation 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%.
A list of 20 drugs from different classes including, sulfonamides, tetracyclines, macrolides, β- Lactam , quinolones and illegal antibiotics such as chloramphenicol was selected that are reported in European Commission Directives 3770/90/EEC and which is listed in annex IV in Council Directive 23/96/EC. The optimization parameters were studied to obtain the proper conditions of the instrument in terms of best sensitivity with lowest interference. The method performance characteristics is tested based on Commission Decision 2002/657/EC by measuring linearity, accuracy, repeatability, within-laboratory reproducibility, decision limit (CCα) and detection capability (CCβ) using LC-MSMS with electrospray ionization. Limit of quantification was 25 ug/kg for all drugs and 0.1 ug/kg for chloramphenicol with accepted mean recoveries ranged from 77-91 and CV% less than 13.
Also, heavy metals were studied as a source of fish contamination. An easy and optimized method was developed using atomic absorption spectrometer after microwave digestion for determination of 11 element including Pb, Cd, Cu, As, Hg, Zn, Fe, Al, Cr, Mn and Sn. Mean recoveries ranged between 81-117% and CV% was less than 1 for all metals.
The methods performance was extra tested using external proficiency tests to evaluate the compliance with │Z│ score; which showed satisfactory results. The methods were accredited by the Finnish Accreditation Service body (FINAS) according to ISO/IEC 17025.
Thirty four fish samples were subjected to histamine assessment using the validated
Abstract
Other data
| Title | Optimization of The Performance of The Methodologies for Detection of Some Contaminants in Food | Other Titles | تحسين كفاءة طرق تقدير بعض الملوثات فى الغذاء | Issue Date | 2015 |
Recommend this item
Similar Items from Core Recommender Database
Items in Ain Shams Scholar are protected by copyright, with all rights reserved, unless otherwise indicated.