Application Notes: LC-MS
On-line SPE-LC of Catecholamines in Urine with Fluorescence Detection
December 2nd 2009Catecholamines 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..
Rapid Screening of Pesticides Using U-HPLC/MS
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.
TSK-GEL Amide-80 HILIC Columns for the Analysis of Melamine and Cyanuric Acid in Milk by LC–MS-MS
June 1st 2009Melamine 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.
Melamine and Cyanuric Acid Detection in 5 Minutes using LC–MS
March 2nd 2009Since 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.
Identification of Psychotropic Substances in Mushrooms by UHPLC–MS
March 2nd 2009Forensic 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.
Determination of Trifluoroacetic Acid Using Ion Chromatography Mass Spectrometry
February 1st 2009Perflourinated 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.
Application of a GPC-LC–MS/MS Method for the Determination of 31 Mycotoxins in Edible OIls
February 1st 2009Gel 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.
TSK-GEL Amide-80 HILIC Columns for Analyzing Melamine and Cyanuric Acid in Milk by LC–MS-MS
February 1st 2009Melamine 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.
Identification of Psychotropic Substances in Mushrooms by UHPLC/MS
February 1st 2009Forensic 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.
Melamine and Cyanuric Acid Detection in 5 Min Using LC–MS
February 1st 2009Since 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).
A Highly Sensitive Method for the Analysis of Tamsulosin (Flomax) in Human Plasma
December 2nd 2008A highly sensitive analytical method for the analysis of tamsulosin in human plasma has been developed for use in bioanalytical studies. The solid-phase extraction (SPE) and UPLC–MS–MS methodologies are described, as well as performance against validation parameters.
maXis High Resolution LC–MS Makes the Most of Ultrafast LC Separations
December 2nd 2008An ultrafast gradient LC separation method was developed to separate a 5-component drug mixture in 30 seconds, with peak widths of 1 second. maXis mass accuracy at sub-ppm levels and true isotopic pattern of the spectra from the peaks lead to a confident elemental formula assignment for each drug compound with the SmartFormula algorithm.