Melamine and Cyanuric Acid in Foodstuffs and Pet Food: Method Validation and Sample Screening

Hazardous levels of melamine in food and feed products have been of great concern after the outbreak of contamination reported in Chinese commodities in 2008. Despite the existence of several analytical methods for melamine (MEL) detection in food, few provide a full validation data set, especially when MEL and cyanuric acid (CYA) are analyzed simultaneously. The aim of this study was to validate an analytical methodology for MEL and CYA analysis in foodstuffs by GC-MS after trimethylsilylation with N,O-bis(trimethylsilyl)trifluoroacetamide. Linearity was obtained in the range of 0.4 to 800 mg/kg for both compounds, with limits of detection (LODs) of 0.15 and 0.05 mg/kg for MEL and CYA, respectively. Screening in 20 food products [3 soya milk powder, 1 baby milk powder, 3 soya powder, 13 diversified cookies and biscuits (8 from China and 2 from Portugal), and 3 dog food) revealed MEL incidence in 55% of the cases, with a maximum concentration of 3.4 mg/kg. CYA was not detected in all samples.     

Rapid Methods in Analytical Chemistry

This article presents the most recent research in analytical chemistry concerning the development of rapid methodologies covering the period from 2009 up until today. In this context, different useful analytical methods have been developed based mainly on typical techniques such as gas chromatography, liquid chromatography, mass spectrometry, electrophoresis, electroanalytical chemistry, and biosensors. The analytical features of these methods have allowed the analysis of samples of different natures, such as environmental, food, pharmaceutical, and biological type, in which wide classes of analytes are promptly determined. The main advantages of these methods are included and discussed in this review regarding novelty, rapidity, sensitivity, selectivity, and costs. It is concluded that the development of rapid methods is still a growing trend in analytical chemistry and that gas- and liquid-chromatography mainly coupled to different modes of mass spectrometry are the most common analytical techniques applied today. Regarding the matrices analyzed, most of the methods have been developed for food analysis, followed by biological and environmental matrices.     

Enhanced Quality Control of Recycled Paperboard for Food Packaging

A method is reported for the industrial quality control of recycled paperboard for food contact applications. Benzophenones, phthalates, and diisopropyl naphthalene were selected as contamination markers. These compounds are commonly found in recycled paperboard packaging and are known to migrate even into dry nonfatty foods. The method was used to analyze commercial recycled board and involved sample pretreatment by accelerated solvent extraction, evaporation, and purification of the extract, and analysis by gas chromatography–mass spectrometry. The accelerated solvent extraction yields were compared with those obtained by Soxhlet extraction and extraction by immersion, and the recoveries of optimized procedures were estimated. The optimized method showed good repeatability, intermediate precision, and sensitivity. Because of the simplicity and partial automation, this method has potential application for the characterization of recycled paperboard.     

Simultaneous Determination of Preservatives,Artificial Sweeteners,and Synthetic Dyes in Kimchi by Ultra-Performance Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometry (UPLC-ESI-MS/MS)

Abstract

A simple and rapid method was developed for the simultaneous determination of five preservatives, six artificial sweeteners, and nine synthetic dyes in kimchi using ultra-performance liquid chromatography electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) with multiple reaction monitoring (MRM). The chromatographic separation was performed in 5.5?min using an Acquity UPLC BEH C18 column (100?mm × 2.1?mm, 1.7?µm) with a mobile phase composed of 0.002% trifluoroacetic acid and 10?mM aqueous ammonium acetate or 9:1 (v/v) methanol:acetonitrile. Linear calibration curves were obtained with correlation coefficients above 0.98. The limits of quantification ranged between 0.227 and 8.569?ng/mL, while the recovery values in kimchi samples were from 83.1 to 113.5%. Forty kimchi samples were analyzed for the food additives, with sweeteners detected in more than half of these samples. The most commonly detected sweetener was saccharin, and six of the kimchi samples contained a combination of sweeteners; dulcin, sucralose, acesulfame K, preservatives, and synthetic dyes were not detected. Based on these results, the developed method can be used for the rapid quality control of food additives in kimchi.     

Monitoring multi-class pesticide residues in fresh fruits and vegetables by liquid chromatography with tandem mass spectrometry

A new analytical method was developed using liquid chromatography with tandem mass spectrometry for the routine analysis of 31 multi-class pesticide residues and applied to approximately 50 fresh fruit and vegetable samples (green bean, cucumber, pepper, tomato, eggplant, watermelon, melon and zucchini). Extraction of the pesticides with ethyl acetate was carried out. The optimal ionisation conditions were selected for each pesticide in the same run. The procedure was validated and the values of some merit figures, such as recovery, precision, linear range, detection limit and quantification limit for each pesticide were calculated together with its calculated expanded uncertainty (U). The average recoveries in cucumber obtained for each pesticide ranged between 74 and 105% at two different fortification levels (n = 10 each) that ranged between 9 and 250 ng g(-1) (depending on the pesticide). The uncertainty associated to the analytical method was lower than 23% for all compounds tested. The calculated limits of detection and quantitation were typically <1 ng g(-1) that were much lower than the maximum residue levels established by European legislation.     

液相色谱-同位素稀释串联质谱法测定动物源性食品中硝基呋喃类代谢物残留

加入同位素标记物的动物源性样品(龙虾、肠衣),在酸性条件下用2-硝基苯甲醛,使样品中呋喃唑酮、呋喃西林、呋喃它酮、呋喃妥因实现衍生。经乙酸乙酯提取浓缩、用甲醇水溶液溶解过滤后,滤液用液相色谱-串联质谱定量。在0.5,1.0和2.0μg/kg3个浓度水平上进行添加回收试验,回收率为80.1％～92.2％,检出限(LOQ)...     

液体顶空-气相色谱法测定食品接触苯乙烯聚合物中单体及溶剂残留

提出了液体顶空-气相色谱法测定食品接触苯乙烯聚合物中残留单体及溶剂的方法。采用N,N-二甲基乙酰胺溶解聚合物,使其中残留单体及溶剂完全释放,并在优化的工作条件下,以基体匹配校正法绘制工作曲线,有效消除基质效应。7种分析物检出限(3S/N)在0.2～4.1mg.kg-1之间。测得方法的回收率在93.2%～103.2%之间,测定值的相对标准偏差(n=6)在1.1%～5.6%之间。     

Polymers and paper as packaging materials of irradiated foodAn NMR study

Effects of γ-irradiation on synthetic polymers and paper used as packaging materials for irradiated food have been studied by NMR. Polystyrene, polybutadiene and some copolymers were studied before and after the γ-irradiation treatment and in the presence or absence of antioxidants and stabilisers. In the absence of additives, the effect of γ-irradiation on polystyrene is negligible even irradiating at high doses. In turn, the role of antioxidants and stabilisers is crucial in polybutadiene and butadiene-containing copolymers. Wood pulp paper was also studied by NMR. Preliminary measurements on γ-irradiated wood pulp sheets show a shortening in the T₂ relaxation time component due to the bound water, i.e. some of the bound water is lost.     

Application of a rapid screening method to detect irradiated meat in Brazil

Based on the enormous potential for food irradiation in Brazil, and to ensure free consumer choice, there is a need to find a convenient and rapid method for detection of irradiated food. Since treatment with ionising radiation causes DNA fragmentation, the analysis of DNA damage might be promising. In this paper, the DNA Comet Assay was used to identify exotic meat (boar, jacaré and capybara), irradiated with ⁶⁰Co gamma rays. The applied radiation doses were 0, 1.5, 3.0 and 4.5 kGy. Analysis of the DNA migration enabled a rapid identification of the radiation treatment.     

Ultraviolet detection of amino acids based on their on-column conjugation with cupric cation using a disposable electrophoresis microdevice

A method for fast sensitive ultraviolet detection of amino acids was developed with a disposable electrophoresis microdevice. The microdevice was conveniently constructed by fixing a fused-silica capillary with a sampling fracture to a printed circuit board. During the separation process, the on-column conjugation of amino acids with cupric cation led to the ultraviolet absorption at 232 nm that could be directly used for fast analysis of amino acids. Using 20 mM boric acid (pH 5.3) containing 5 mM cupric cation and 0.015% Tween 20 as running buffer, this method could completely separate lysine, glutamine and serine at a sampling time of 2 s at +210 V and a separation voltage of +1800 V (240 V/cm). The theoretical plate numbers were from 140,000 to 205,000 plates/m. The linear ranges were from 10 to 500 μM for lysine, 20-1000 μM for glutamine and serine. The novel protocol had been successfully used to detect amino acids in beverage samples with recovery more than 85.0%, indicating its advantages and potential analytical application in different fields.