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1.
Inorg Chem ; 63(10): 4502-4510, 2024 Mar 11.
Artigo em Inglês | MEDLINE | ID: mdl-38408375

RESUMO

A fast, sensitive, selective, and biocompatible dual sensor of an antineoplastic medication (methotrexate) and a neurotransmitter (adrenaline) is still being searched by present-day scientists. To overcome this issue, we have designed a functionalized, robust, bio-friendly luminescent MOF for the sensitive, selective, and rapid monitoring of methotrexate and adrenaline. This probe is the first ever reported MOF-based fluorescence sensor of methotrexate and second only for adrenaline. This fluorescence probe has a very low limit of detection (LOD) of 0.34 and 11.2 nM for adrenaline and methotrexate, respectively. The sensor can detect both the targeted analytes rapidly within 5 s. It can also detect adrenaline and methotrexate from human blood serum and urine accurately and precisely. This reusable sensor is equally efficient in detecting methotrexate from environmental water specimens. Biocompatible, user-friendly, and inexpensive chitosan@MOF@cotton composites were fabricated for the detection of adrenaline and methotrexate from the nanomolar to the micromolar range by the naked eye under a fluorescence lamp. This probe displayed high reproducibility, precision, and accuracy in sensing methotrexate and adrenaline. Fluorescence resonance energy transfer (FRET) and the inner filter effect (IFE) are the possible mechanisms for adrenaline and methotrexate sensing, respectively. The possible mechanism was supported by using required instrumental techniques and theoretical simulations.


Assuntos
Antineoplásicos , Metotrexato , Humanos , Água , Reprodutibilidade dos Testes , Epinefrina , Neurotransmissores
2.
J Chromatogr A ; 1716: 464645, 2024 Feb 08.
Artigo em Inglês | MEDLINE | ID: mdl-38219625

RESUMO

Alkylphosphonofluoridic Acids (APFA) are the major thermal degradation products of G- and A-series nerve agents and thus play a vital role in the verification analysis of Chemical Weapons Convention. Present study focuses on the development of sample clean-up, derivatization procedures and gas chromatography tandem mass spectrometric analysis of APFA in aqueous samples. APFA were found to be much more delicate than the corresponding alkylphosphonic acids and thus required subtle optimizations. Retention of analytes on silica and polymer-based anion exchangers followed by elution under alkaline conditions yielded best recoveries. Elution under acidic conditions led to partial or complete degradation of the analytes to alkylphosphonic acids. Silylation reactions, particularly with MTBSTFA were found the best in terms of chromatographic responses and resolution of the derivative peaks. Methylations with diazomethane, which requires acidic reaction media, failed to produce desired yields of the derivatives. Under optimized conditions, the analytes produced the recoveries ranging from 76.9 to 94.5% with RSD ≤9.2%. The best LOD's in the tandem mass spectrometric analysis ranged from 13 to 56 ng/ml. The applicability of the method was tested by spiking the analytes in the retained aqueous samples received for the 52nd proficiency test conducted by the Organization for the Prohibition of Chemical Weapons (OPCW).


Assuntos
Substâncias para a Guerra Química , Agentes Neurotóxicos , Agentes Neurotóxicos/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Substâncias para a Guerra Química/análise , Limite de Detecção , Espectrometria de Massas em Tandem , Ácidos , Água/química
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