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1.
Acta Chim Slov ; 69(1): 49-59, 2022 Mar 15.
Artigo em Inglês | MEDLINE | ID: mdl-35298022

RESUMO

An HPLC-UV/FLD method for simultaneous detection of ten antibiotics in surface waters was developed. Antibiotics were extracted from water using solid phase extraction. An Atlantis T3 column was used with acetonitrile and 0.05% trifluoroacetic acid as a mobile phase for separation, with a total running time of 45 min. Signal detection was performed at 280 nm; fluoroquinolones were additionally quantified by fluorescence detection. Validation parameters such as linearity, recovery and precision were evaluated. The limits of detection (LOD) in river waters were in the range 0.1-1.3 µg/L for antibiotics detected by UV, and 0.039 and 0.073 µg/Lfor fluoroquinolones detected by FLD. LOD are sufficiently low to consider this method as a first alternative for HPLC-MS methods that will allow alerting for the presence of antibiotics in surface waters. This screening method is rapid, sensitive, reproducible and economical.


Assuntos
Antibacterianos , Poluentes Químicos da Água , Cromatografia Líquida de Alta Pressão/métodos , Espectrometria de Massas , Extração em Fase Sólida/métodos
2.
J Food Sci ; 86(4): 1296-1305, 2021 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-33733483

RESUMO

At present, screening of active ingredients from natural products for pharmacological and clinical research is mostly time-consuming and costly. In this study, a molecular network (MN) guided high performance liquid chromatography-ultraviolet-fluorescence detector (HPLC-UV-FLD) method was carried out to profile the global antioxidant activity compounds, including the trace amount ingredients in Camellia nitidissima Chi (CNC). Firstly, HPLC-UV-FLD postcolumn derivatization system was utilized to screen the antioxidants. Then the MN of CNC was established via mass spectrometry (MS) data for getting the connection between ingredient structures. As a result, HPLC-UV-FLD indicated three antioxidant ingredients: gallic acid (126.3 mg/g), catechin (564.8 mg/g), and salicylic acid (24.3 mg/g). Combined with the MN, the actives' precise location and connection relationship were clarified based on the structural similarities. A new antioxidant ingredient, okicamelliaside, was suggested and evaluated at free radical scavenging and enzymatic protection. The novel method of activity and structural correlation analysis based on MN could provide a useful guide for screening trace active ingredients in natural products. PRACTICAL APPLICATION: Three main ingredients were screened out from Camellia nitidissima Chi by HPLC-UV-FLD postcolumn derivatization system. Integrated molecular network and HPLC-UV-FLD analysis, a new type of antioxidant okicamelliaside was selected. The novel method of activity and structural correlation analysis based on molecular network could provide a useful guide for screening trace active ingredients in natural products.


Assuntos
Antioxidantes/análise , Camellia/química , Cromatografia Líquida de Alta Pressão/métodos , Chás de Ervas/análise , Catequina/análise , Fluorescência , Ácido Gálico/análise , Espectrometria de Massas , Extratos Vegetais/química , Ácido Salicílico/análise
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