April 5th 2024
In the present study, a gradient reversed-phase high-performance liquid chromatography (RP-HPLC) method has been designed and validated to quantify ornidazole (OZ) in the marketed formulation (oral gel) with the application of QbD.
Low-Level Determination of Mutagenic Nitrosamine Impurities in Drug Substances by LC–MS/MS
July 12th 2021This article discusses the development of a series of applications that will allow for the determination of a number of nitrosamines that have been identified by the FDA as genotoxins to monitor, initially showing how to perform a separation of these compounds from the API and then looking at how MS can be applied to the analysis to ensure that the required detection limits can be reached.
Decomposing animal tissue releases volatile organic compounds (VOCs), of interest in forensic science. We describe the use of GC×GC–qMS/FID retrofitted with a reverse fill/flush (RFF) flow modulator for analyzing these VOCs in a tropical climate.
Online Hydrophobic Interaction Chromatography–Mass Spectrometry (HIC–MS) Analysis of Proteins
February 1st 2021Recent advances in stationary phases for hydrophobic interaction chromatography (HIC) permit HIC–MS analysis of intact antibodies and other proteins using direct flow to the mass spectrometer.
Ultra-Sensitive and Rapid Analysis of Per- and Polyfluoroalkyl Substances (PFAS) in Water
February 1st 2021A method is described using a triple quadrupole LC–MS instrument with isotopic dilution to obtain the highest accuracy and confidence for analysis of per- and polyfluoroalkyl substances (PFAS) in water. Excellent method spike recoveries and robustness were found in wastewater.
Not (Only) Reversed-Phase LC–MS: Alternative LC–MS Approaches
September 1st 2020In many applications, LC–MS approaches using HILIC, SFC, SEC, IEC, and HIC offer advantages over conventional reversed-phase LC–MS. The examples presented here should inspire you to consider these options for your analyses.
Low-pressure gas chromatography (LPGC)–MS should be the first option in many GC–MS applications to provide fast, sensitive, and robust analyses; and the installation, instrumentation, and implementation of LPGC is possible in any GC–MS system.
Quantification of European Union (EU)-priority polycyclic aromatic hydrocarbons (PAHs) in plant matrices is a crucial task. Various methods for enrichment and preconcentration, such as the preloaded-pipette tip solid‑phase extraction (SPE) (1), are available. Nevertheless, analyte recovery as a result of homogenization, sample preparation, and extraction are rarely discussed in the field of phytopharmacy. This study deals with the recovery in dry plant extracts, which are typically used in phytopharmaceuticals and reflect the actual polycyclic aromatic hydrocarbon content in the commercially available end product (2). The aim of this study was to monitor benzo[a]pyrene, benzo[a]anthracene, chrysene, and benzo[b]fluoranthene loss of spiked samples as a result of commonly-used sample pretreatment, extraction, filtering, and evaporating techniques in 1:1 (v/v) cyclohexane–ethyl acetate primulae flos and sambuci flos dry extracts. Results showed that improper sample preparation can lead to false results. In the case of benzo[a]pyrene with a deviation of 155% from the theoretical true value.
A Simple LC–MS Multi-Analyte Method to Determine Food Additives and Caffeine in Beverages
June 30th 2020A simple LC–MS method has been developed and validated for the simultaneous determination of 18 synthetic food additives and caffeine in soft and energy drinks, and in various alcoholic beverages. Nine food colours (tartrazine, sunset yellow FCF, azorubine, ponceau 4R, allura red AC, patent blue V, brilliant blue FCF, green S, brilliant black BN), two preservatives (sorbic and benzoic acid) and seven sweeteners (acesulfame K, aspartame, cyclamic acid, saccharin, sucralose, neohesperidin DC, neotame) were targeted food additives. The method employs reversed-phase ultra-high performance liquid chromatography (UHPLC) for analyte separation and a single quadrupole mass spectrometer for their detection. The limits of quantification were low enough to enable a reliable control of maximum limits set for some additives (Regulation [EC] No. 1333/2008). The method was applied for analysis of a wide range of samples collected at a typical supermarket: 14 soft drinks, 19 energy drinks, and 43 alcoholic beverages.
Determination of PAHs in Combustion-Related Samples via Multidimensional Chromatographic Methods
December 1st 2019Gas chromatography–mass spectrometry (GC–MS), reversed-phase LC with stop-flow fluorescence (FL), and constant energy synchronous fluorescence spectroscopy (CESFS) are explored to determine PAH isomers in three combustion-related standard reference materials.
Clinical Metabolomics: Expanding the Metabolome Coverage Using Advanced Analytical Techniques (NA)
December 1st 2019Clinical metabolomics requires analytical methods that provide both high resolution and high throughput. In this review, we assess the promise of a variety of techniques-including HILIC, SFC, multidimensional LC, ion-mobility mass spectrometry, and data-independent acquisition mass spectrometry methods-to meet those needs.
The versatile size-exclusion ultrahigh-performance liquid chromatography (SE-UHPLC) platform method described here provides superior separation for bispecific monoclonal antibody formats compared to a previous method.