Mass Spectrometry

Gas chromatography–mass spectrometry (GC–MS) and liquid chromatography–mass spectrometry (LC–MS) techniques offer advantages in separating and confirming the identity of constituents in novel psychoactive substances.

Accurate-mass approaches offer a significant advance over nominal-mass approaches in the arena of qualitative analysis, and some of the analytical approaches can now be conducted in a relatively routine manner.

A study of colony collapse disorder in honey bees illustrates how mass spectrometry–based proteomics techniques can be used to to identify pathogens without any prior knowledge of what is contained in the sample.

A proof-of-concept application for detecting abused steroids in urine samples collected from an antidoping surveillance program

An update on the sample preparation and LC–MS-MS tools available for allergen detection, as well advantages of those techniques.

A summary of the most recent advances in sample preparation, instrumentation, and data-processing techniques for MALDI-IMS

A discussion of active pharmaceutical ingredient (API) selection, drug product development, and mass spectrometry instrumentation

A review highlighting the combination, or potential combination, of various separation methods with ambient ionization mass spectrometry

How to create a liquid chromatography–tandem mass spectrometry (LC–MS-MS) system using mass spectrometers, a high performance liquid chromatography (HPLC) binary pump system, and an autosampler

A breakthrough using a microfluidic interface to conduct sensitive time-of-flight secondary ion mass spectrometry (TOF-SIMS) analysis and study liquid surfaces in situ under vacuum conditions is described here.

A critical look into the future of imaging mass spectrometry is made by addressing some of the fundamental and technical challenges that still need to be overcome.

A method is illustrated for the simultaneous analysis of ethyl glucuronide and ethyl sulfate in human urine samples.

The combination of GC with time-of-flight (TOF)-MS proves to be a successful approach for the challenging analysis of persistent organic pollutants in complex matrices such as sediment and fish samples.

This study illustrates the versatility of a laser-induced acoustic desorption (LIAD) approach for volatilization of analytes in modern mass spectrometry.

High-definition screening by gas chromatography–mass spectrometry (GC–MS) is shown to be a viable option for the reliable identification of odorous compounds in pork.

Ion mobility–mass spectrometry (IM-MS) is outlined as a separations method, several examples of the utility of IM-MS for complex biological measurements are illustrated, and the implications of this approach for systems biology research are discussed.

Identifying unknown compounds continues to challenge analysts.

On the 50th anniversary of the invention of the laser, Michael Balogh examines its importance in MS practice.

In mass spectrometry, the electrospray ionization technique quickly earned its place among the primary analytical tools. Yet it is not always the best tool for the job.

With the advances in LC-MS in recent years, is there another practical option on the horizon for those who need the specificity of MS and can justify the narrow definition of a purpose-built system?

This month's installment addresses some elementary aspects of the mass spectrum, the tools employed by the experienced practitioner, and advances being made into identifying unknowns.

Michael Balogh uses examples such as the recent acetonitrile shortage to examine the topic of "the unknowable" as it pertains to separation science.

Mass spectrometry-based electronic nose technology (MS-nose technology) is a fast hyphenated technique for digital odour characterization of food and beverage products.

Part 2 of this three-part series focuses on comparing operation and performance of the most well known mass spectrometers.

Researchers at the University of Utah's (Salt Lake City) Sports Medicine Research and Testing Laboratory developed a test for testosterone and epitestosterone in urine that uses liquid chromatography with tandem mass spectrometry detection (LC-MS-MS).

Ramipril impurities D and E are well-known degradation products of ramipril in the finished dosage form. A significant amount of an additional impurity was detected in ramipril tablets by an isocratic reversed-phase high performance liquid chromatography (HPLC) method on a short column. The structure of this impurity was proposed based on liquid chromatography–mass spectrometry (LC–MS) data using an electron spray ionization source. Structural elucidation using nuclear magnetic resonance (NMR) and infrared (IR) spectroscopy was facilitated by a newly developed preparative isolation method. This impurity was characterized as (2R,3aR,6aR)-1-[(R)-2-[[(R)-1-(ethoxycarbonyl)-3-phenylpropyl]amino]propanoyl]octahydrocyclopenta[b]pyrrole-2-carboxylic acid (impurity L). Its identification, synthesis and characterization are discussed.

Over the last 10 years, several solvent-free microextraction techniques for gas chromatography (GC) and mass spectrometry (MS) have been developed. Two of these techniques, solid-phase microextraction (SPME) and stir-bar sorptive extraction (SBSE), are available commercially for the analysis of volatile compounds, such as flavors in foods and beverages, and toxic organic compounds in environmental applications. Other techniques, such as open tubular trapping, inside needle capillary adsorption trap (1), in-tube SPME, capillary microextraction, needle trap, and headspace solid-phase dynamic extraction (2), were also developed for different applications. The basic principle for all of these techniques is essentially the same. Volatile and semivolatile compounds are adsorbed on a sorbent coating, often packed on the interior surface of a capillary column or stainless steel needle. After the sample is concentrated on the coating, the compounds are desorbed thermally in the heated injection port of a gas..

Automated solid-phase extraction (SPE) has been used extensively with liquid chromatography–tandem mass spectrometry (LC–MS-MS) to facilitate high-throughput analysis in the pharmaceutical, diagnostic, and forensic toxicology areas. In this work, we demonstrate the use of a systemized approach to SPE method development and LC–MS-MS analysis. This approach provides dramatic savings in analysis time and takes advantage of new innovations in high performance liquid chromatography (HPLC) columns to provide the cleanest extracts for LC–MS injection.

Illegal drug use worldwide is at an all-time high. There is a crucial need for fast and accurate analysis to positively identify suspected drugs in criminal investigations. Gas chromatography combined with time-of-flight mass spectrometry (GC–TOFMS) can be a valuable tool for drug testing in forensic crime laboratories. Method development and GC–TOFMS experimentation was conducted in cooperation with a local crime laboratory. The laboratory testing presented will illustrate highly efficient methods and data developed for crime labs that assist in the battle against illegal drugs. Many drug classes have chemical properties that present particular analytical challenges, such as poor detector response, chemical lability, or poor chromatographic peak shape. This article presents GC–TOFMS methods developed for several major drug classes and chemical functionalities. The major drugs included in the initial method development are methamphetamine, ecstasy, and heroin. Robust and accurate..

A summary of the five-day mass spectrometry conference held this month in Denver, Colorado.