Application Notes: Food and Beverage

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The Application Notebook

The FDA has no objection to Rebaudioside A having a generally recognized as safe (GRAS) status as a sweetener for food and drink.1 Stevia sweeteners may contain other steviol glycosides as well, mainly Stevioside, Rebaudioside C and Dulcoside A. Because the FDA GRAS confirmation is only for the use of Rebaudioside A at 95% purity or above in food and beverages, stevia extracts must be highly purified and characterized prior to use.

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The Application Notebook

The screening of pesticides, mycotoxins, and veterinary drugs is of great importance in regulated environments such as food or feed analysis. Due to some of the limitations of traditional triple quadrupole approaches (for example, targeted analyte detection, limited number of compounds, and unidentified unknown compounds), there is currently a trend towards use of full-scan MS data for the analysis of residue samples. Current screening approaches mainly rely on the use of ToF instruments coupled to U-HPLC delivering mass accuracy (~5 ppm) at a maximum resolution of <15,000. This can produce inaccurate mass measurements due the presence of unresolved background matrix interferences. In this work we show a full-scan MS screening approach with the Thermo Scientific Exactive mass spectrometer, a novel single-stage Orbitrapâ„¢ MS capable of providing precise mass accuracies at resolutions of up to 100,000 without the need for internal mass calibration.

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The Application Notebook

Since melamine and its metabolites are extremely polar compounds, they serve as very good candidates for HILIC chromatography. Simultaneous and fast determination and confirmation of melamine and cyanuric acid along with two other compounds using a novel amino bonded phase in HILIC mode coupled with a complete solutions approach is presented.

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The Application Notebook

Melamine is an organic base and a trimer of cyanamide, with a 1,3,5-triazine skeleton. Melamine can react with formaldehyde to produce melamine resin, a very durable thermosetting plastic, and melamine foam, a polymeric cleaning product. Some end products made from melamine include countertops, dry erase boards, fabrics, glues, housewares, and flame retardants. Melamine is also one of the major components in Pigment Yellow 150, a colorant in inks and plastics.

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The Application Notebook

An Agilent ZORBAX Rapid Resolution HT Eclipse Plus Phenyl-Hexyl column resolved many compounds from Stevia rebaudiana Bertoni plant extracts using an isocratic reversed phase method with UV and MS detection instead of a typical approach employing an amino column with a refractive index or other special detector. The Eclipse Plus Phenyl-Hexyl method's advantages include high peak capacity, isocratic mobile phase, low acetonitrile consumption, and MS compatibility.

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The Application Notebook

The United States Food and Drug Administration (U.S. FDA) and the European Union (EU) have published regulations and provided guidance on the use of chemicals in food packaging materials. Tekmar provides method parameters for the HT3â„¢ Automated Headspace Analyzer for the determination of VOCs that may be contained in food contact packaging materials under various conditions. Temperature and mixing parameters were investigated to determine which VOCs may be released when subjected to these conditions.

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The Application Notebook

Simulated Moving Bed technology (SMB) is a continuous chromatography technique widely used in the pharmaceutical/biotechnology industry. The continuous chromatographic separation of sodium sulphate (Na2 SO4) from a mixture of glucose and mannose was established by using the Orochem Zuccheroâ„¢ columns and the SMB technology. The main advantages of SMB over batch chromatography includes better yields, higher purity, and decreased solvent usage, which together make the SMB technology economically viable and ideal for desalting applications.

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The Application Notebook

Based on the QuEChERS AOAC Official Method 2007.01, sixteen pesticides were used for evaluating the performance of the Agilent's AOAC Buffered Extraction and SampliQ QuEChERS Dispersive SPE kits for General Fruits and Vegetables. Apple was selected as the fruit matrix. The pesticides are from the "representative pesticides" list (1). A method working well for these representative pesticides should work equally well for the other pesticides that are routinely monitored in multi-class, multi-residue methods. The compounds are from nine different pesticide classes: including acidic, basic, neutral, base-sensitive, and acid-labile pesticides. The selected pesticides are suitable for LC–MS-MS analysis. The MRLs of these pesticides have been set at 10 ng/g or higher (2–4).

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The Application Notebook

Since September 2008, 294 000 infants and young children suffered urinary problems as a result of the contamination of melamine in infant milk powder and were hospitalized. This hospitalization was required to treat the symptoms caused by the ingestion of melamine contaminated infant formula and related dairy products. Previously in 2007, pet food, animal feed wheat gluten and other protein-based foods were found to contain residues of melamine and its degradation product cyanuric acid.

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The Application Notebook

GC–MS method is presented for the quantitative determination and confirmation of melamine residues in milk products. The milk sample was cleaned up using Agilent's SampliQ SCX SPE cartridges before derivatization. The derived extracts were analysed by GC–MS with EI in synchronous SIM/scan mode on a Agilent J&W DB-5ms Ultra Inert column.

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The Application Notebook

Penicillins are regulated substances in food for human consumption. The minimum residue limits range from 1 ng/g to as high as 50 ng/g depending on the compound. Because of the complexity of food matrices measuring the level of contaminants requires a total solution composed of sample extraction, sample clean-up, chromatographic separation and detection. In this paper, a solid-phase extraction method with a high performance liquid chromatography tandem mass spectrometry method (HPLC–MS–MS) is shown for the simultaneous determination of six antibiotic residues.

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The Application Notebook

Gel Permeation Chromatography (GPC) is widely used for sample clean up in mycotoxin analysis. The most commonly described methods use GPC columns packed with SX-3 BioBeads suitable for cleaning Zearalenone, Aflatoxins, and Trichothesenes from edible oils and fatty matrices. Separation of Fumonisins from the oil fraction are inadequate with this column.

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The Application Notebook

The recent establishment of a 1 μg/g safety threshold for melamine in infant foods has led to an immediate need for more sensitive methods. Here we established GC–MS conditions for highly reproducible analyses and evaluated the effectiveness of both solvent-based and matrix-matched standards. Using this method, melamine and cyanuric acid were reliably detected at and below 1 μg/g in infant formula.

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The Application Notebook

Run a difficult food sample on your IC and you stand a big chance that you will wreck the column. Of course, you can waste a lot of time on tedious sample preparation steps to eliminate undesired matrix components. Or you can go for Metrohm's automated compact stopped-flow dialysis providing optimum separation while protecting your column from detrimental compounds.

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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

Melamine is an organic base and a trimer of cyanamide, with a 1,3,5-triazine skeleton. Melamine can react with formaldehyde to produce melamine resin, a very durable thermosetting plastic, and melamine foam, a polymeric cleaning product. Some end products made from melamine include countertops, dry erase boards, fabrics, glues, housewares, and flame retardants. Melamine is also one of the major components in Pigment Yellow 150, a colorant in inks and plastics.

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The Application Notebook

LC–MS-MS instruments operating in Multiple Reaction Monitoring (MRM) are widely used for targeted quantitation on triple quadrupole and hybrid triple quadrupole linear ion trap (QTRAP® ) systems because of their well known selectivity and sensitivity. In MRM mode, the first quadrupole (Q1) filters a specific precursor ion; the collision cell (Q2) generates fragments (product ions) which are filtered in the third quadrupole (Q3). Although this double mass filtering greatly reduces noise there is always a chance that elevated background levels or matrix signals interfere with the targeted analyte.

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The Application Notebook

The global economic downturn, particularly the collapse of the automotive and associated industries, has caused an overall reduction in the demand for acrylonitrile. Since acetonitrile is obtained as a co-product in the production of acrylonitrile, the pharmaceutical, food, environmental, and chemical industries are experiencing an unprecedented acetonitrile shortage. This shortage has resulted in a sharp price increase, in some cases as much as 6-8 times; and the price is projected to remain high even after the production returns to normal.

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The Application Notebook

Since September 2008, 294,000 infants and young children suffered urinary problems due to the contamination of melamine in infant milk powder and were hospitalized. This hospitalization was required to treat the symptoms caused by the ingestion of melamine contaminated infant formula and related dairy products. Previously in 2007, pet food, animal feed, wheat gluten, and other protein-based foods were found to contain residues of melamine and its degradation product cyanuric acid (2).

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The Application Notebook

The analysis of chemical residues in food requires techniques sensitive enough to detect and quantify contaminants at or below the maximum residue limit (MRL) of the compound in a given sample matrix. Because of increased food safety regulations and the growing numbers of samples to be analyzed, it is critical that the analytical techniques provide high sample throughput.

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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

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

The recent development of ultra-HPLC (UHPLC) has provided a great potential for high throughput analysis achieved using small (sub-2 μm) particle size columns at increased linear velocities. The advantage of UHPLC over conventional HPLC is increased throughput without sacrificing resolution. Despite their popularity, sub-2 μm particle columns impose practical difficulties, such as high backpressure (which often requires a UHPLC system) and susceptibility to column fouling. Thus difficulty can be overcome using 2.0 to 2.5 μm particles. This study describes an example (analysis of vanilla extract) of transferring a conventional LC method to a high-throughput method using newly developed Acclaim® RSLC 2-μm columns that are based on spherical, porous, high-purity silica particles (dp = 2 μm, pore size = 120 Å, surface area = 320 m2/g).