This review discusses the integration of liquid chromatography (LC), mass spectrometry (MS), and nuclear magnetic resonance (NMR) in the comprehensive analysis of small molecules from complex matrices. We first discuss the steps taken toward making the three technologies compatible, so as to create an efficient analytical platform. The development of online LC-MS-NMR, highlighted by successful applications in the profiling of highly concentrated analytes (LODs 10 μg) is discussed next. This is followed by a detailed overview of the alternative approaches that have been developed to overcome the challenges associated with online LC-MS-NMR that primarily stem from the inherently low sensitivity of NMR. These alternative approaches include the use of stop-flow LC-MS-NMR, loop collection of LC peaks, LC-MS-SPE-NMR, and offline NMR. The potential and limitations of all these approaches is discussed in the context of applications in various fields, including metabolomics and natural product discovery.
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http://dx.doi.org/10.1002/mas.21575 | DOI Listing |
Anal Chim Acta
February 2025
Food Inspection and Quarantine Technology Center of Shenzhen Customs, Shenzhen Academy of Inspection and Quarantine, Shenzhen, 518045, PR China.
Background: Ochratoxin A (OTA) is toxic secondary metabolites produced by fungi and can pose a serious threat to food safety and human health. Due to the high stability and toxicity, OTA contamination in agricultural products is of great concern. Therefore, the development of a highly sensitive and reliable OTA detection method is crucial to ensure food safety.
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January 2025
Departamento de Ciencias Preclínicas, Facultad de Medicina, Universidad de La Frontera, Temuco 4811230, Chile.
Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) is a well-known technique for polymer analysis, particularly for determining the molecular weight and structural details of dendrimers. In this study, we evaluated the performance of various matrices, such as 2',4',6'-trihydroxyacetophenone (THAP), α-cyano-4-hydroxycinnamic acid (HCCA), and sinapinic acid (SA), and their combinations, on the sensitivity and resolution of poly(amidoamine) (PAMAM) dendrimers of different generations (G3.0, G4.
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January 2025
Department of Materials Science and Engineering, Iowa State University, Ames, IA 50011, USA.
This review examines the recent advancements and unique properties of polymer-inorganic hybrid materials formed through coordination bonding (Class II hybrids), which enable enhanced functionality and stability across various applications. Here, we categorize these materials based on properties gained through complexation, focusing on electrical conductivity, thermal stability, photophysical characteristics, catalytic activity, and nanoscale self-assembly. Two major synthetic approaches to making these hybrids include homogeneous and heterogeneous methods, each with distinct tradeoffs: Homogeneous synthesis is straightforward but requires favorable mixing between inorganic and polymer species, which are predominantly water-soluble complexes.
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January 2025
Department of Bioproducts and Biosystems Engineering, University of Minnesota, St. Paul, MN 55108, USA.
Emerging contaminants (ECs), encompassing pharmaceuticals, personal care products, pesticides, and industrial chemicals, represent a growing threat to ecosystems and human health due to their persistence, bioaccumulation potential, and often-unknown toxicological profiles. Addressing these challenges necessitates advanced analytical tools capable of detecting and quantifying trace levels of ECs in complex environmental matrices. This review highlights the pivotal role of mass spectrometry (MS) in monitoring ECs, emphasizing its high sensitivity, specificity, and versatility across various techniques such as Gas Chromatography-Mass Spectrometry (GC-MS), Liquid Chromatography-Mass Spectrometry (LC-MS), and High-Resolution Mass Spectrometry (HR-MS).
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January 2025
Department of Chemistry, Faculty of Sciences and Mathematics, University of Niš, Višegradska 33, 18000 Niš, Serbia.
Species of the genus are known for their pharmacological properties and essential oils, the chemical composition of which remains inadequately studied. In this work, GC-MS analysis, synthesis, and spectral techniques (UV, IR, MS, and NMR) were employed to identify 83 constituents in the essential oil from roots, which accounted for 98.1% of the total GC-peak area.
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