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
Biotherapeutics must endure in-depth testing to validate their efficacy and safety before their release to the medical community. Characterization and quantitation of these large molecule medicines is traditionally performed with ligand binding assays or radiolabeling procedures. Issues with selectivity, accuracy, and unavailability of applicable assays for the characterization and quantitation of certain biotherapeutics means that liquid chromatography–mass spectrometry (LC–MS) is becoming an increasingly selected method for biotherapeutics testing. Typically used for small molecules, LC–MS can be adapted for larger molecule analysis with additional high throughput and multiplexing capabilities. New method development has turned LC–MS into a highly sensitive option for biotherapeutics validation.
The analysis of pesticide residues in food samples from the state of Connecticut's regulatory monitoring program are compared to USDA and US FDA results.
This application note demonstrates the use of the Thermo Scientific Syncronis C18 1.7 ?m column for the determination of esomeprazole by UHPLC-UV.
The Column spoke to Evelien Dejaegere from Waters Corporation about the method life cycle management approach and its importance in the pharmaceutical sector.
The method described here is a simple method for detection of a wide spectrum of metals and for quantitative analysis over a wide dynamic range of elements, including both toxic metals and those metals essential for health and well-being.
Through a Q & A format, this article illustrates some of the uses of CE in this area.
Combining a membrane with a solid sorbent can improve selectivity and save time in sample preparation.
A look at how the concentration of essential oils in cedar leaves is affected by changes in temperature and the amount of rainfall
This study demonstrates that GC–TOF-MS can be a useful approach to generate comprehensive fragrance profiles of essential oils. Peak deconvolution enables discrimination between closely eluted compounds, and soft electron ionization, assisted by comparison of ion ratios, makes it possible to discriminate between isomeric monoterpenes with very similar mass spectra at conventional 70-eV ionization energies.
In this article, the sensitivity of two-dimensional gas chromatography coupled to two different detectors - a time-offl ight mass spectrometer (GCXGC–TOF-MS) and a fl ame ionization detector (GC?GC–FID) - was compared to the sensitivity of conventional one-dimensional gas chromatography (GC–TOF-MS and GC–FID) by determining method detection limits (MDLs) for a series of different compounds with different polarities.
A dedicated GC– MS analyser was developed to address the increasing need for more sensitive catalyst poisoner analysis. The system combines the separation power and robustness of a classic backflush configuration with the selectivity and sensisitivitiy of mass spectrometry.
It is hypothesized that in particular cases, conventional planar chromatography provides a more effective and robust system than column chromatography with regard to separation efficiency and peak distribution of mixtures composed of low-retarded analytes. Under similar reversed-phase experimental conditions, a regular distribution of thin-layer chromatography (TLC) spots of four natural estrogens (estetrol, estriol, 17?-estradiol, and estrone) corresponds to strong irregular dispersion of peaks in chromatograms generated by high performance liquid chromatography. In both cases, the efficiency of separation was assessed using simple optimization criteria such as selectivity (?min) and resolution (Rs min). The distribution of chromatographic spots was evaluated using the relative resolution product (r). The results revealed that an excellent separation of the components of interest could be achieved easily using simple nonforced and isocratic TLC. Such an interesting property of planar chromatography is mainly driven by the nonlinear relationship between k and Rf retention factors. This article also reports the practical advantages of TLC for the separation of estrogenic steroid mixtures at different temperatures.
Can databases of column characteristics be used to help with HPLC column selection ahead of method development?
Quinine- and quinidine-derived anion-exchanger chiral stationary phases have proven to be versatile in enantiomer separation of acidic compounds in HPLC. In this article, the authors demonstrate their performance in specific HPLC applications involving enantiomer resolution and topoisomer separation.
Urinary excretion profiling is a key element in the pharmokinetic characterization of new chemical entities (NCEs). Recent advances in ultra-high performance liquid chromatography (UHPLC) column technology offer improved results for liquid chromatography tandem mass spectrometry (LC–MS¬–MS) analysis, enabling rapid quantification of specific drugs and their metabolites in biological matrices.
The aim of this work was to find the optimal conditions to achieve sufficient limits of detection (LOD) that would permit the detection of neurotransmitters by LC–MS–MS in biological samples. An optimized HILIC–ESI–MS–MS system for the analysis of the 12 selected compounds was proposed.
This application demonstrates that stringent sensitivity requirements for the detection of potentially harmful primary aromatic amines can be fulfilled when using an Agilent 1290 Infinity LC system equipped with the 1290 large volume injection kit.
The use of electrospray ionization–mass spectrometry for rapid and specific determination of the widely used metal deactivators Irgamet-30 and Irgamet-39 is demonstrated here.
Many workers in pharmaceutical laboratories are unable to change any aspect of their methods, although they often encounter severe problems and create many out-of-specification (OoS) results. They are particularly afraid to investigate these problems from a chromatographic perspective in case they generate new unforeseen problems. In the literature, however, there are numerous examples showing that it is worthwhile trying to understand the reasons for “unexplainable” behaviour in ultrahigh-pressure liquid chromatography (UHPLC) using modelling. By using modelling, problems can be recognized and often eliminated with legal operations according to the allowed tolerance limits mentioned in pharmacopoeia descriptions. The following article aims to show that “visual chromatographic modelling” can be a useful aid.
A sensitive method that reduces the number of false-positive results
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.
An analysis of the capabilities of direct analysis in real time (DART) and desorption electrospray ionization (DESI) sources for the analysis of contaminated fabrics
A review highlighting the combination, or potential combination, of various separation methods with ambient ionization mass spectrometry
Automated column and mobile phase screening is the current trend in the pharmaceutical industry to develop chiral methods. This study presents comprehensive strategies for automated rapid chiral HPLC method development including normal-phase, reversed-phase and polar organic phase separation modes.
Automated column and mobile phase screening is the current trend in the pharmaceutical industry to develop chiral methods. This study presents comprehensive strategies for automated rapid chiral HPLC method development including normal-phase, reversed-phase and polar organic phase separation modes.
The development of various analytical MS methods to investigate the chemical composition of liquids used in electronic cigarettes and characterize their quality is presented in this study.