PharmTech LCGC Sciex Webinar 11.10

Food and Beverage Analysis

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Researchers from the Swedish University of Agricultural Sciences (Uppsala, Sweden) and the University of Tabriz (Tabriz, Iran) developed a solid-phase extraction method to separate sterol oxidation products in food lipids for analysis by gas chromatography (GC) and GC?mass spectrometry.

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The Application Notebook

Melamine is an industrial chemical with a high nitrogen content that can cause kidney stones and lead to renal failure. In some instances, melamine has been added to baby formula and dairy products as a substitute for protein. This paper presents an efficient and definitive gas chromatography–mass spectrometry (GC–MS) method to identify melamine and related compounds based on the released US Food and Drug Administration (FDA) method.

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The Application Notebook

This application details a fast, reliable and highly selective trace-level screening method for the quantification of polychlorinated biphenyls (PCBs) in environmental, food and biological samples, using gas chromatography and a triple stage quadrupole mass spectrometer. The analytical strategy is analogous to the well-established US Environmental Protection Agency (USEPA) Method 1668A.

A research group from the University of La Laguna and ICIA (both in La Laguna, Tenerife, Canary Islands, Spain) used multiwalled carbon nanotubes as a solid-phase extraction (SPE) medium for extracting eight organophosphorus pesticides from various commercial apple, grape, orange, and pineapple juices.

Researchers from the University of Barcelona (Barcelona, Spain) and Arboriculura Mediterranea Mas de Bover (Tarragona, Spain) implemented a factorial experimental design in developing a solid-phase microextraction (SPME)?gas chromatography (GC)?mass spectrometry (MS) method to analyze volatile phenols in virgin olive oils.

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Special Issues

With the globalization of trade, food production and distribution have become truly international businesses. When we dine out, the fish might come from Japan, the rice from Australia, the spices from China, and the strawberries from Mexico. We take it for granted that the food we eat is safe and free from contamination that could make us seriously ill.

Researchers at the University of Castilla-La Mancha (Spain), Ecole Nationale des Sciences Appliquees (Agadir, Morocco), and Institut Agronomique et Veterinaire Hassan II (Agadir, Morocco) developed a method for screening paraquat and diquat in olive oil samples.

E-Separation Solutions

American and European Foulbrood in honeybees is caused by two bacterial species, Paenibacillus larvae and Melissococcus pluton, respectively. For control of these bacteria, only a few antibiotics are recommended in Europe and the U.S.A. However, a variety of antibacterial agents are used, the sulfa drugs being the most popular. Residues of these antibiotics are quite often found in honey samples and are of concern to consumers around the world due to toxic or allergic reactions. Earlier sample preparation methods involved using silica-based C18 or neutral polymers as sorbents with an aqueous wash prior to elution of sulfonamides. In this communication, we describe a simple and effective method for cleanup and quantitation of antibacterial sulfonamides from honey using the polymeric strong cation exchange SPE sorbent strata-X-C and a Gemini HPLC column.

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The Application Notebook

In March 2007, several North American manufacturers of pet food voluntarily issued nationwide recall notices for some of their products that were reportedly associated with renal failure in pets. The raw material wheat gluten, used to manufacture the pet food, was imported from China and was identified as the source of contamination.

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The Application Notebook

A new technique, QuEChERS, standing for Quick, Easy, Cheap, Effective, Rugged, and Safe, is readily accepted by both the AOAC International and the Committee of European Normalization (CEN) for the pesticide residues in foods and agriculture products. Waters DisQuEâ„¢ Dispersive Sample Preparation Kit contains conveniently-packaged centrifuge tubes with pre-weighed sorbents and buffers designed for use with the AOAC official QuEChERS methods.

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The Application Notebook

Recent developments in HRes Fast-LC systems have enabled the use of sub-3 μm stationary phases at higher flow rates and elevated pressures. HRes Fast-LC can provide significant improvements in both resolution and throughput.

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The Application Notebook

Organic acids are present in many matrices and play crucial roles. Extensive research involving low molecular mass organic acids (LMMOA) has been performed in food chemistry since these acids contribute to the organoleptic properties of food and beverages, including flavor, color, aroma, taste, shelf-life, and health effects. Developing a profiling method to monitor LMMOA levels in raw materials and final products is very desirable. Many reported methods focus on limited numbers of LMMOAs and are incapable of providing a complete LMMOA profile.

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The Application Notebook

Mycotoxins, toxic secondary metabolites of several fungal species, represent food safety issues of high concern. Deoxynivalenol, the most abundant trichothecene mycotoxin, can be found worldwide as a contaminant of wheat, barley, maize and other cereals (1,2). The transmission of deoxynivalenol from barley into beer has been reported in several studies (3,4). Therefore, its levels should be controlled.

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The Application Notebook

This article describes a straightforward ion chromatographic method that uses isocratic elution and pulsed amperometric detection (PAD) to sensitively determine water-soluble polyols and sugar alcohols as well as mono-, di- and oligosaccharides in essential and nonessential foodstuffs. While carbohydrate determination of most foodstuffs requires only minimal sample pretreatment such as dilution and filtration, samples with interfering matrices such as protein-containing dairy products have to be dialyzed prior to injection.

Researchers from the University of Barcelona (Barcelona, Spain) analyzed heterocyclic amines in meat samples using pressurized liquid extraction followed by liquid chromatography with tandem mass spectrometry detection (LC?MS-MS).

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Special Issues

Over the last 10 years, several solvent-free microextraction techniques for gas chromatography (GC) and mass spectrometry (MS) have been developed. Two of these techniques, solid-phase microextraction (SPME) and stir-bar sorptive extraction (SBSE), are available commercially for the analysis of volatile compounds, such as flavors in foods and beverages, and toxic organic compounds in environmental applications. Other techniques, such as open tubular trapping, inside needle capillary adsorption trap (1), in-tube SPME, capillary microextraction, needle trap, and headspace solid-phase dynamic extraction (2), were also developed for different applications. The basic principle for all of these techniques is essentially the same. Volatile and semivolatile compounds are adsorbed on a sorbent coating, often packed on the interior surface of a capillary column or stainless steel needle. After the sample is concentrated on the coating, the compounds are desorbed thermally in the heated injection port of a gas..

Researchers at the Universit? di Camerino in Camerino, Italy have developed a new GC-MS and LC-MS technique for the determination of five ink photoinitiator residues: 2-isopropylthioxanthone (ITX), benzophenone, 2-ethylhexyl-4-dimethylaminobenzoate (EHDAB), 1-hydroxycyclohexyl-1-phenyl ketone (IRGACURE 184) and ethyl-4-dimethylaminobenzoate (EDAB) in packaged beverages.

Researchers from the Nutrition and Bromatology Group, Analytical and Food Chemistry Department, and Faculty of Food Science and Technology at the University of Vigo (Ourense, Spain) have developed a GC-MS method for determining residues of 12 insecticides and 11 fungicides in leafy vegetables.

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The Application Notebook

Mycotoxins, toxic secondary metabolites of several fungal species, represent food safety issues of high concern. Deoxynivalenol, the most abundant trichothecene mycotoxin, can be found worldwide as a contaminant of wheat, barley, maize and other cereals (1,2). The transmission of deoxynivalenol from barley into beer has been reported in several studies (3,4). Therefore, its levels should be controlled.

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The Application Notebook

Supercritical fluid chromatography (SFC) is a normal phase separation technique. In SFC, supercritical CO2 in combination with one or more polar organic solvents, most commonly alcohols, is used as the mobile phase. Owing to the lack of intermolecular interactions, supercritical fluid typically possesses lower viscosity and higher diffusivity than those solvents used in traditional high performance liquid chromatography (HPLC). This allows for higher flow rates, faster analyses, and the use of longer columns for higher chromatographic efficiencies. Initially deemed a niche chromatographic technique for chiral separation, the horizon of SFC applications has rapidly expanded to include achiral analyses of natural products, biodiesel, oligomer, pesticides/herbicides, and peptides. This is due, in part, to the improvements in detection choices and performances for SFC. Evaporative light scattering detectors (ELSDs) coupled with SFC have found wide use in many pharmaceutical and chemical laboratories (1).

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The Application Notebook

Gel permeation chromatography (GPC) has been used as an effective cleanup procedure for removing high molecular weight interfering molecules such as lipids, pigments, proteins, and polymers before GC or HPLC analysis. The GPC cleanup method has been extensively documented (1–3) and is also recommended in US EPA SW-846 Method 3640A. To demonstrate the efficacy of this method to extract polar and nonpolar substances by using the KNAUER Smartline GPC Cleanup Unit 6500, olive oil samples were investigated by spiking these with different types of organic pollutants, including PAHs, phthalates, phenols, and triazine.