Application Notes: LC-MS

Solvent-reduced determination of 100 contaminants from low double-digit to low triple-digit pg/L in 100 mL surface water samples, meeting the requirements of the EU-WFD based on SBSE-TD-GC-MS/MS

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A rapid, accurate, and reproducible method was developed for high-throughput testing of nicotine, cotinine, trans-3’-hydroxycotinine, nornicotine, norcotinine, and anabasine in urine. Data show that a fast and highly efficient analysis of these basic compounds can be achieved with the Raptor Biphenyl column using standard reversed-phase LC–MS mobile phases that are compatible with a variety of LC–MS instrumentation.

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The term ionic liquid refers to organic salts with relatively low melting points (below 100 °C) that usually consist of an organic cation or anion and a counterion, in either organic or inorganic form. Ionic liquids exhibit unique characteristics such as extremely low vapour pressure, excellent thermal stability, electrical conductivity, a high degree of polarity and miscibility with various types of solvents. Ionic liquids have been used as catalysts and solvents in organic chemistry and electrochemistry and as mobile phase modifiers or functionalized stationary phases in separation science.1–3

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Catecholamines are important markers for the diagnosis and management of tumour diseases of the sympathoadrenal system. The major catecholamines are dopamine, norepinephrine and epinephrine. Urine tests have shown to be applicable to measure the level of catecholamines in the human body. Various separation methods have been used for the clean-up of catecholamines in biological fluids: solvent extraction, adsorption on alumina, ion-exchange and solid-phase extraction of a diphenylboronic acid-catecholamine complex. From the point of simplicity, reproducibility and automation the last method is the most suitable and can be realized by on-line SPE–LC. Diphenylborate forms a negatively charged complex with the diol groups of catecholamines. These complexes which are strongly retained on a polystyrene-divinylbenzene cartridge in alkaline medium (pH 8.5) can be eluted in a second step from the SPE unit directly onto the HPLC column. The separation of catecholamines is performed in isocratic mode by..

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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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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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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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Tobacco Specific Nitrosamines (TSNA) are a group of carcinogens found only in tobacco products and are formed from nicotine and related alkaloids during the production and processing of tobacco and tobacco products (1). Due to their carcinogenic properties, efforts have been made to reduce TSNA levels in tobacco products. The project goal was to demonstrate a high throughput and sensitive method to monitor TSNA levels.

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Morphine is an effective pain-relieving drug that is primarily metabolized into morphine-3-glucuronide (M3G) and morphine-6-glucuronide (M6G). The highly potent M6G may have adverse effects, such as respiratory depression and renal failure, if accumulated in the body. As morphine abuse continues to affect modern society, an effective method must be established to analyse morphine and its structurally related compounds in biological fluid samples. In this work, a UPLC–MS-MS method was developed to separate six morphine-related compounds on a 2.1 Ã- 100 mm, 1.8 μm ACQUITY UPLC HSS T3 column in a single run using an ACQUITY UPLC system connected to a fast-scanning triple-quadrupole MS detector (TQD). The method achieved adequate retention of these very polar compounds by reversed-phase (RP) chromatography in an 8-min total run time.

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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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Forensic laboratories face a daunting task to identify trace amounts of controlled substances in small samples of seized evidence. Unambiguous identification is required to meet the stiff challenge that is sure to be raised in the courtroom. Positive proof is especially difficult to establish if the controlled substance is hidden in a complex food matrix with a high content of sugars, fats, fatty acids, proteins and alkaloids.

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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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Perflourinated organic acids are ubiquitous and found at relatively low concentrations in the environment (1). Trifluoroacetic acid (TFA) is the persistent atmospheric degradation product of hydrofluorocarbons (HFCs) that are increasingly used as an alternative to banned, ozone-damaging chlorofluorocarbons (CFCs). However, debate surrounds the use of HFCs because of their potential to contribute to global warming and demonstrated toxicity to the environment (2). TFA is also widely used in pharmaceutical and biotechnology purification processes. It is crucial to monitor for TFA in environmental risk assessment and in products intended for human use. TFA can be measured by gas chromatography (GC) after sample preparation and chemical derivatization (3), ion chromatography (IC) (4), and capillary electrophoresis (5). This paper describes an IC-MS method to separate TFA from common anions based on Reagent-Freeâ„¢ IC (RFICâ„¢) technology with sensitive and selective mass spectrometric detection.

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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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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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Forensic laboratories face a daunting task to identify trace amounts of controlled substances in small samples of seized evidence. Unambiguous identification is required to meet the stiff challenge that is sure to be raised in the courtroom. Positive proof is especially difficult to establish if the controlled substance is hidden in a complex food matrix with a high content of sugars, fats, fatty acids, proteins, and alkaloids.