Application Notes: Sample Prep

Using a targeted solid phase extraction (SPE) method and GC–ECD analysis, chlorinated pesticides are extracted from poultry fat resulting in a method that decreases the amount of labor and reagents when compared to the USDA-FSIS CHC2 method.

A simple, automatable cleanup method is developed for the analysis of acrylamide from coffee, yielding absolute recoveries that exceed 92% when analyzed by LC–MS-MS.

Using a targeted solid phase extraction (SPE) method and GC–ECD analysis, chlorinated pesticides are extracted from poultry fat resulting in a method that decreases the amount of labor and reagents when compared to the USDA-FSIS CHC2 method.

A simple, automatable cleanup method is developed for the analysis of acrylamide from coffee, yielding absolute recoveries that exceed 92% when analyzed by LC–MS-MS.

Cannabinoids are successfully extracted from a complex brownie matrix using the QuEChERS sample preparation technique, significantly reducing the presence of matrix interferences. The resulting clean samples are analyzed by GC–MS using a specialized deactivated GC column to provide heightened peaks for the cannabinoid compounds.

EPA Method 625 is greatly simplified by using solid phase extraction (SPE) as an alternative to traditional liquid-liquid extraction (LLE). Using this SPE technique, paired with a sensitive GC–MS analysis, increases throughput and data quality, while decreasing manual labor and solvent usage.

Cannabinoids are successfully extracted from a complex brownie matrix using the QuEChERS sample preparation technique, significantly reducing the presence of matrix interferences. The resulting clean samples are analyzed by GC–MS using a specialized deactivated GC column to provide heightened peaks for the cannabinoid compounds.

Improving and optimizing EPA Method 593 using solid phase extraction (SPE) enhances sensitivity and maximizes efficiency while screening by LC–MS-MS for different female birth control hormones present in drinking and waste water.

EPA Method 625 is greatly simplified by using solid phase extraction (SPE) as an alternative to traditional liquid-liquid extraction (LLE). Using this SPE technique, paired with a sensitive GC–MS analysis, increases throughput and data quality, while decreasing manual labor and solvent usage.

Phospholipid removal proves to yield superior results as compared to a traditional protein precipitation step when analyzing a complex plasma matrix via LC–MS-MS. The results displayed a decrease in ion suppression, increased analyte sensitivity, and an improvement in column lifetime.

Enhancing the extraction of vitamins A and E in serum using simplified liquid extraction (SLE) significantly improves the LC–MS-MS detection of target compounds, all while preserving a simple and robust method.

Phospholipid removal proves to yield superior results as compared to a traditional protein precipitation step when analyzing a complex plasma matrix via LC–MS-MS. The results displayed a decrease in ion suppression, increased analyte sensitivity, and an improvement in column lifetime.

Enhancing the extraction of vitamins A and E in serum using simplified liquid extraction (SLE) significantly improves the LC–MS-MS detection of target compounds, all while preserving a simple and robust method.

Using oral fluid as the matrix, a viable and simple solid phase extraction method for a wide range of drugs is developed. Several oral fluid collection devices were evaluated to determine the effectiveness of the cleanup procedure, ultimately confirming that the method is both robust and widely applicable.

Improving and optimizing EPA Method 593 using solid phase extraction (SPE) enhances sensitivity and maximizes efficiency while screening by LC–MS-MS for different female birth control hormones present in drinking and waste water.

Using oral fluid as the matrix, a viable and simple solid phase extraction method for a wide range of drugs is developed. Several oral fluid collection devices were evaluated to determine the effectiveness of the cleanup procedure, ultimately confirming that the method is both robust and widely applicable.

An ultra-sensitive sample preparation technique using solid phase extraction (SPE) microelution 96-well plates effectively concentrates peptides and allows for cleanup of small volume.

A suite of unknown drug compounds from whole blood are analyzed by LC–MS-MS, requiring the need for an effective yet nonspecific cleanup technique. The resulting method demonstrates a simple and fast sample preparation procedure that is suitable for screening many compounds.

A suite of unknown drug compounds from whole blood are analyzed by LC–MS-MS, requiring the need for an effective yet nonspecific cleanup technique. The resulting method demonstrates a simple and fast sample preparation procedure that is suitable for screening many compounds.

An ultra-sensitive sample preparation technique using solid phase extraction (SPE) microelution 96-well plates effectively concentrates peptides and allows for cleanup of small volume.

SPME-GC–MS with on-column injection can be successfully employed for flavour profiling of food samples. The on-column injector of the GC-2010 can be used for SPME without any modifications, only an external ring adapter was used to facilitate the injection. The data can be compared with sensorial data of food.

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..

The use of EVOLUTE CX mixed-mode columns provides high and consistent recoveries across a range of complex matrices, from biological fluids to milk products. The dual retention mechanism ensures that matrix components such as proteins, salts and phospholipids are removed, resulting in lower ion suppression and accurate analysis.

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.

Human health not only depends on providing good medical care, but also on the priority given to prevent exposure to environmental and other health risks. Persistent Organic Pollutants (POPs) are organic compounds typically of anthropogenic origin that resist degradation and accumulate in the food chain and are associated with adverse effects on human health and the environment (1). Due to their toxicity to humans, at much lower concentration than other pollutants, it is important to monitor compounds like polychlorinated dioxins/furans PCDD/Fs, DLPCBs, BDEs, and PCNs. More sophisticated requirements are needed for their analysis. In the past, extraction and clean-up of POPs present in fish and biota samples were conducted with procedures such as Soxhlet extraction, acid digestion, and liquid-liquid extraction. The clean-up of these samples was accomplished through chromatographic columns using different types of adsorption media such as silica, alumina, and carbon. These analytical methods used for analysis..

In U.S. EPA Method 5035 there are two collection options for samples containing high levels of volatile organic compounds (VOCs). The first involves collecting a bulk soil sample in the field. In the lab, the bulk soil is dispersed in a water miscible solvent. Next, an aliquot of the solution is added to 5 mL of water and finally, the sample is purged. The second option is to collect a 5 g soil sample and add it to a pre-weighed vial containing a prescribed amount of water miscible solvent. An aliquot is then purged. Both of these processes are time consuming and have the potential to introduce human error both in the field and in the laboratory.

Polysaccharide-based chiral stationary phases (CSP) are successfully employed to achieve the majority of analytical and preparative enantioselective separations. However, there are a number of separations where significant modification or enhancement of selectivity is necessary. Two new columns, CHIRALPAK AY-H and CHIRALCEL OZ-H, have been introduced to meet these needs.

LC/GC approaches to analysis are attractive because they combine the selectivity of solid-phase sorbents in the first dimension with the separating power and peak capacity of capillary GC in the following dimensions.

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.

EPA Method 8260 is used to determine volatile organic compounds (VOC's) in a variety of matrices including ground and surface waters. This method is commonly used in environmental laboratories where gas chromatography (GC), mass spectrometry (MS) and purge and trap (P&T) technology are used for the analysis and subsequent detection of VOC's.