Determination of melamine in feed: Validation of a gas chromatography–mass spectrometry method according to 2004/882/CE regulation

Squadrone, Stefania; Ferro, Gian Luca; Marchis, Daniela; Mauro, Carolina Saori Ishii; Palmegiano, P.; Amato, Giuseppina; Génin, Eric; Abete, Maria Cesarina

doi:10.1016/j.foodcont.2009.10.013

Cited by 43 publications

(30 citation statements)

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“…All raw materials such as fish meal (54 %), barley (11 %), soybean meal (12 %), corn gluten meal (12 %), cod liver oil (6 %), vitamin supplement (0.5 %), mineral supplement (0.5 %) and binder (lignosulfonates, 4 %) were previously tested negative for triazines (Squadrone et al 2010), and then weighed, mixed and prepared in batches. Then, triazines were added and mixed with the raw materials to create nine experimental diets containing 250, 500 and 1,000 mg of MEL or CYA per kilogram of feed or 250, 500 and 1,000 mg each of MEL and CYA per kilogram of feed.…”

Section: Experimental Designmentioning

confidence: 99%

Melamine–cyanurate complexes and oxidative stress markers in trout kidney following melamine and cyanuric acid long-term co-exposure and withdrawal

Pacini

Dörr

Elia

et al. 2014

Fish Physiol Biochem

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In 2007, renal failure and death in pets were linked to pet food containing both melamine (MEL) and cyanuric acid (CYA). In mammals and fish, the co-administration of MEL and CYA causes renal crystal formation. Moreover, little is known about the process of crystal removal in fish. The aim of this study was to evaluate the formation of MEL-cyanurate crystals in kidney of rainbow trout (Oncorhynchus mykiss) fed combined MEL and CYA diets for 10 weeks at 250, 500 and 1,000 mg/kg in feed (equivalent to 2.5, 5, 10 mg/kg body weight of trout fed 1 % body weight per day). During the exposure trial and throughout a withdrawal period, prooxidant effects of MEL and CYA were evaluated on oxidative stress markers such as catalase, glutathione S-transferase and malondialdehyde. Crystal formation was dose and time dependent, and after six withdrawal weeks, crystals persisted in kidney of trout treated the highest triazine dose. Catalase and glutathione S-transferase activity in kidney of trout exposed to both triazines for 10 weeks indicated that MEL (with or without CYA) can exert a higher prooxidant effect than CYA dispensed singly. Although the enzymes activity increase appears to be reverted after two MEL withdrawal weeks, persistence of crystals may lead to severe damage in renal cells of fish.

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Section: Experimental Designmentioning

confidence: 99%

Melamine–cyanurate complexes and oxidative stress markers in trout kidney following melamine and cyanuric acid long-term co-exposure and withdrawal

Pacini

Dörr

Elia

et al. 2014

Fish Physiol Biochem

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“…Although methods have been utilized to detect MEL, not all of these are satisfactory. For example, high-performance liquid chromatography alone [17][18][19] or combined with tandem mass spectrometry (MS/MS), [18][19][20] gas chromatographymass spectrometry, 21 capillary electrophoresis, 22 infrared spectroscopy, 23,24 and nuclear magnetic resonance spectroscopy 25 are highly sensitive but require complicated pretreatment procedures and expensive instruments and equipment. Moreover, most of these tests require large amounts of organic solvents that are dangerous to user health and harmful to the environment.…”

Section: Introductionmentioning

confidence: 99%

Lateral flow test strip based on colloidal selenium immunoassay for rapid detection of melamine in milk, milk powder, and animal feed

Wang¹,

Zhi²,

Zhao³

et al. 2014

IJN

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Although high melamine (MEL) intake has been proven to cause serious health problems, MEL is sometimes illegally added to milk products and animal feed, arousing serious food safety concerns. A satisfactory method of detecting MEL in onsite or in-home testing is in urgent need of development. This work aimed to explore a rapid, convenient, and cost-effective method of identifying MEL in milk products or other food by colloidal selenium-based lateral flow immunoassay. Colloidal selenium was synthesized by L-ascorbic acid to reduce seleninic acid at room temperature. After conjugation with a monoclonal antibody anti-MEL, a test strip was successfully prepared. The detection limit of the test strip reached 150 μg/kg, 1,000 μg/kg, and 800 μg/kg in liquid milk, milk powder, and animal feed, respectively. No cross-reactions with homologues cyanuric acid, cyanurodiamide, or ammelide were found. Moreover, the MEL test strip can remain stable after storage for 1 year at room temperature. Our results demonstrate that the colloidal selenium MEL test strip can detect MEL in adulterated milk products or animal feed conveniently, rapidly, and sensitively. In contrast with a colloidal gold MEL test strip, the colloidal selenium MEL test strip was easy to prepare and more cost-efficient.

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“…The fatty acid mix standard solution, containing palmitic, stearic, oleic and linoleic acids, was analyzed as much as 1 mL. LOD was calculated as 3 SD, while LOQ was calculated as 3.3 LOD (Squadrone et al, 2010).…”

Section: Instrument Performance Analysismentioning

confidence: 99%

Evaluation of Major Fatty Acids Determination in Palm Oil by Gas Chromatography-Flame Ionization Detection

2016

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The fatty acid composition of palm oil is the major factor influencing its physical and chemical properties. The purpose of this research was to evaluate the analytical performance of major fatty acids (palmitic acid, stearic acid, oleic acid, and linoleic acid) analysis in palm oil. Triglycerides of palm oil were derivatized to fatty acid methyl esters (FAMEs) by using boron trifluoride (BF 3 ) in methanol. FAMEs were determined by gas chromatography-flame ionization detection (GC-FID) using DB-23 capillary column as stationary phase. The studied parameters were instrument performance analysis, the efficiency of fatty acid derivatization, stability of derivatized analytes, accuracy, repeatability, intra-lab reproducibility, ruggedness, and method uncertainty. The evaluation results showed the instrument linearity at a working range of 5 to 40 mg/mL marked by coefficient of determination (R 2 ) between 0.991-0.995. Instrument limits of detection (LOD) and instrument limits of quantification (LOQ) for 4 major fatty acids analysis were 26-35 µg/mL and 86-128 µg/mL, respectively. The increase of fatty acid concentration led to the decrease of derivatization efficiency in the fatty acids analysis. The result also showed that derivatized analytes were stable during 24 h storage at freeze temperature. The average recovery values by spiking method with the spiking concentration at 50 and 90 mg/g sample were at 75-94 % for stearic and linoleic acids analysis, however those for palmitic and oleic acids analysis were considered very low (<40 %), due to their low derivatization efficiency. Repeatability and intra-lab reproducibility of 4 major fatty acids analysis were at acceptable ranges, 0.45-1.38 % and 1.15-2.03 %, respectively. Determination by varying the volume of derivatizing agent showed the rugged method. Uncertainty of repeatability (U r ) and uncertainty of reproducibility (U r ) were ranged at 1.84-9.02 mg/g and 1.40-10.65 mg/g, respectively. This method was considerably reliable for the analysis of less abundance fatty acids in palm oil, stearic and linoleic acids.

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Determination of melamine in feed: Validation of a gas chromatography–mass spectrometry method according to 2004/882/CE regulation

Cited by 43 publications

References 1 publication

Melamine–cyanurate complexes and oxidative stress markers in trout kidney following melamine and cyanuric acid long-term co-exposure and withdrawal

Melamine–cyanurate complexes and oxidative stress markers in trout kidney following melamine and cyanuric acid long-term co-exposure and withdrawal

Lateral flow test strip based on colloidal selenium immunoassay for rapid detection of melamine in milk, milk powder, and animal feed

Evaluation of Major Fatty Acids Determination in Palm Oil by Gas Chromatography-Flame Ionization Detection

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