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1.
J Chromatogr A ; 1609: 460512, 2020 Jan 04.
Article in English | MEDLINE | ID: mdl-31542208

ABSTRACT

The simultaneous use of nitrite and sorbate as preservatives in meat products may produce mutagenic compounds such as the ethylnitrolic acid and 2-methyl-1,4-dinitro-pyrrole. We developed a sensitive analytical method with high metrological reliability. After assessing several extraction approaches and chromatographic separation modes, a modified Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) approach was chosen for sample preparation, which were analyzed by reversed-phase liquid chromatography (with C18 as stationary phase) coupled to tandem mass spectrometry. After validation, we confirmed that this method is fit-for-purpose, since it was applied to the analysis of several meat products. Limits of detection were set from 5 to 20 µg kg-1. Satisfactory results were obtained for both compounds, such as precision (CV > 20%) and recoveries (77-92%). This method determine these carcinogenic compounds in processed meats, contributing to the preservation of public health and the improvement of food regulation and control.


Subject(s)
Analytic Sample Preparation Methods , Hydroxylamines/analysis , Meat Products/analysis , Mutagens/analysis , Nitriles/analysis , Pyrroles/chemistry , Tandem Mass Spectrometry/methods , Calibration , Chromatography, Liquid , Chromatography, Reverse-Phase , Reproducibility of Results
3.
Talanta ; 185: 151-159, 2018 Aug 01.
Article in English | MEDLINE | ID: mdl-29759182

ABSTRACT

The use of sorbate and nitrite in meat processing may lead to the formation of 2-methyl-1,4-dinitro-pyrrole (DNMP), a mutagenic compound. This work was aimed at developing and validating an analytical method for the quantitation of DNMP by liquid chromatography-tandem mass spectrometry. Full validation was performed in accordance to Commission Decision 2002/657/EC and method applicability was checked in several samples of meat products. A simple procedure, with low temperature partitioning solid-liquid extraction, was developed. The nitrosation during the extraction was monitored by the N-nitroso-DL-pipecolic acid content. Chromatographic separation was achieved in 8 min with di-isopropyl-3-aminopropyl silane bound to hydroxylated silica as stationary phase. Samples of bacon and cooked sausage yielded the highest concentrations of DNMP (68 ±â€¯3 and 50 ±â€¯3 µg kg-1, respectively). The developed method proved to be a reliable, selective, and sensitive tool for DNMP measurements in meat products.


Subject(s)
Meat Products/analysis , Mutagens/analysis , Pyrroles/analysis , Chromatography, High Pressure Liquid , Spectrometry, Mass, Electrospray Ionization , Tandem Mass Spectrometry
4.
Bioorg Med Chem ; 15(24): 7553-60, 2007 Dec 15.
Article in English | MEDLINE | ID: mdl-17889546

ABSTRACT

In the present paper 12 N-quinolin-8-yl-arylsulfonamides synthesized by coupling 8-aminoquinolines with various arylsulfonylchlorides were assayed in vitro against Leishmania amazonensis, Leishmania chagasi and Trypanosoma cruzi strains. This series of new compounds were found to be selective for Leishmania spp. promastigote and amastigote forms. The most active compound was the N-(8-quinolyl)-3,5-difluoro-benzenesulfonamide 10 with an IC(50) against L. amazonensis and L. chagasi of 2.12 and 0.45 microM, respectively. The less cytotoxic biphenyl derivative 7 was very effective against intracellular L. amazonensis with a reduction of macrophage cell infection of 82.1% at 25 microM. In addition, a copper complex 17 of an inactive ligand was readily synthesized and showed high leishmanicidal and trypanocidal activity against both extra and intracellular forms.


Subject(s)
Leishmania/drug effects , Quinolines , Sulfonamides , Trypanocidal Agents/chemical synthesis , Trypanosoma cruzi/drug effects , Animals , Antiprotozoal Agents/chemical synthesis , Antiprotozoal Agents/chemistry , Antiprotozoal Agents/pharmacology , Copper/chemistry , Inhibitory Concentration 50 , Molecular Structure , Organometallic Compounds/chemical synthesis , Organometallic Compounds/chemistry , Organometallic Compounds/pharmacology , Parasitic Sensitivity Tests , Quinolines/chemical synthesis , Quinolines/chemistry , Quinolines/pharmacology , Sulfonamides/chemical synthesis , Sulfonamides/chemistry , Sulfonamides/pharmacology , Trypanocidal Agents/chemistry , Trypanocidal Agents/pharmacology , Zinc/chemistry
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