Application Notes

Increased temperature has been used to assist the elimination of organic modifier required in the mobile phase, to achieve analyte separation in pure aqueous mobile phases.

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.

LC–GC approaches to analysis are particularly attractive because they combine the selectivity of solid phase sorbents in the first dimension with the separating power and peak capacity of a capillary GC column in the following dimensions. Their widespread use is limited because of the difficultly in desolvating the stream from the LC dimension without the solvent vapour passing down the GC column in significant quantity. An alternative approach to elution chromatography in the first dimension is to harness the specificity of the solid-phase process for digital chromatography using discontinuous changes in solvent polarity. Digital chromatography on a small sorbent bed reduces the volume of mobile phase to discrete plugs that are sufficiently small to be injected directly into a GC with a large volume injector or, alternatively, subsampled into a conventional split/splitless injector.

Using HILIC with highly efficient ethylene bridged hybrid (BEH) particles results in faster methods that exhibit improved polar retention, higher sensitivity, enhanced chromatographic resolution, and significantly improved column lifetime.

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.

To meet the growing need for fast reversed-phase enantiomer separations, two new 3-μm reversed-phase columns, CHIRALCEL® OD® -3R and CHIRALPAK® AD® -3R, have been introduced. High column performance and column stability under a wide range of conditions, including aqueous solvent systems suited to LC–MS, have been

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.

The Pirkle - Type Whelk-O®1 CSP is a synthetically made chiral selector covalently bonded to a silica support. This phase is well known in the industry for its broad degree of generality, mobile phase compatibility, and ability to invert elution order. Most commonly used polysaccharide coated CSP's are sensitive to the presence of certain mobile phase modifiers such as DEA, TEA, and TFA. Retained memory effects can adversely affect a separation resulting in broad and tailing peaks, no peak elution, and reduced or loss of separation altogether. To remove these unwanted memory effects, the column must be rinsed with an alcohol, such as methanol or ethanol. This is a time consuming and costly process. The Whelk-O®1 CSP does not exhibit any such retained memory behavior.

The Clean Air Act (CAA) (1) provides the U.S. Environmental Protection Agency authority to enforce regulations limiting emissions of volatile organic compounds (VOCs) and other air pollutants. The Compendium of Methods for the Determination of Toxic Compounds in Ambient Air includes a variety of sampling and analysis methods (2, 3), including use of single- and multi-sorbent tubes. Concentrating a large volume of sample onto a sorbent tube, followed by thermal desorption onto a GC column provides an efficient, cost-effective means of monitoring VOCs at parts per billion (ppb) or parts per trillion (ppt) levels.

The new reversed-phase ProSwift® 1 mm i.d. column is a divinylbenzene-based monolithic column for routine chromatography of proteins and other biomolecules. It is available in two different lengths. The shorter (1 Ã- 50 mm) format is designed for fast separations and the longer (1 Ã- 250 mm) format is intended for high resolution analytical separations. However, depending on the application, either can be used for separation of proteins and for coupling with mass spectrometry.

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.

Hydrogen, commonly used as a carrier gas instead of Helium for gas chromatography (GC) can be supplied via cylinders or by the electrolysis of water using an in-house generator containing metallic electrodes or an ionomeric membrane. An in-house generator can provide a significant increase in safety and convenience with a reduction in operating costs.

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).

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.

Hydroxyethylstarches (HES) are used increasingly as plasma expanders in medical applications. The HES' circulation time in the blood depends strongly on its molar mass distributions. Historically, polysaccharide characterization by Gel Permeation Chromatography (GPC) has been problematic, especially

Heparin is well-known as an anti-coagulant, antithrombotic drug. Chemically, it is a linear polysaccharide that is derived from animal tissues. For some time it has been known that heparin is not a homogeneous substance; rather, it is a heterogeneous mixture of molecules ranging in molar mass from less than 5,000 to more than 30,000 Daltons. Heparin can be chemically or enzymatically depolymerized to obtain low molecular weight (LMW) heparin products, which exhibit an improved pharmacological profile.

The CUSTODIONâ„¢ solid phase microextraction (SPME) syringe was used to rapidly sample and concentrate volatile organic compounds (VOCs) from water in 5 s. The VOCs were analyzed quickly and reliably in approximately 70 s using the GUARDIONâ„¢ -7 portable capillary gas chromatograph toroidal ion trap mass spectrometer (GC-TMS).

Sample preparation is an essential technique to remove unwanted matrix components prior to LC–MS-MS analysis of drugs in biological fluids. Plasma matrix components whether endogenous (salts, proteins, and phospholipids) or exogenous (dosing vehicles, e.g. PEG 400), can interfere with compounds of interest leading to regions of ion suppression or enhancement. This can lead to inaccurate quantitation and have adverse effects on sensitivity. Mixed-mode SPE provides cleaner extracts as a result of rigorous interference wash steps, afforded by the dual retention mechanism of the sorbents.

Asymmetric flow field flow fractionation is a type of field flow fractionation (FFF) separation technique. FFF has been co-existing with size exclusion chromatography (SEC) for several decades.

SCM-4 - The 4th International Symposium on the Separation and Characterization of Natural and Synthetic Macromolecules

Hypercrosslinked polystyrene-type (solid-phase extraction) SPE materials exhibit a unique ability to enter p-interactions with aromatic, heterocyclic and unsaturated compounds. This property permits selective extraction and pre-concentration of the above classes of species from non-polar media and fatty matrices. The principle has been exploited for developing analytical protocols to determine polar furan derivatives in mineral transformer oil, polyaromatic hydrocarbons (PAHs) in smoked fish and for the fractionation of polychlorinated aromatic compounds in environmental matrices.

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.

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.

Goal: Positively identify trace amounts of cannabinoids in a complex food matrix quickly, with minimal sample preparation and no chemical derivatization.

A 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.

An 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.

The success of evaporative light scattering detection relies on evaporating the eluent without destroying the analyte particle. Where the analyte is non-volatile, evaporator temperatures of 50-100 °C can be used without compound degradation, thus giving maximum sensitivity. However, when compounds have high vapor pressures and the eluent has a high boiling point (e.g. water), detection of semi-volatile compounds is problematic, because the evaporation temperature needs to be set at 30 °C or above in order to evaporate the solvent.

The separation and quantitation of drug substances and counterions are two important determinations in the pharmaceutical industry (1). Drug substances and counterions are determined by HPLC (often on reversed-phase columns) and by ion chromatography (IC), respectively. IC is the preferred method for selective and sensitive screening of both cationic and anionic pharmaceutical counterions (2). To increase the analysis throughput, it is desirable that for analysis of drug formulation both drug substance and counterions can be determined within a single run. Naproxen is a non-steroidal anti-inflammatory drug commonly used for treating moderate to severe pain, fever, inflammation, and stiffness. Naproxen sodium was approved by the U.S. Food and Drug Administration (FDA) as an over-the-counter drug. No reports were found describing one technique for the simultaneous determinations of both naproxen and the counterion (Na+).

Improve the separation of 14 drugs of abuse in a complex mixture by employing a ternary solvent gradient.

Studies of odd-electron CID behaviors reveal that free radical fragmentation is structure-dependent and is directly correlated with the functional groups that stabilize the newly-formed free radicals.