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1.
J Chromatogr A ; 1621: 461040, 2020 Jun 21.
Artigo em Inglês | MEDLINE | ID: mdl-32204883

RESUMO

We offer a concept for the simultaneous determination of QuEChERS amenable and highly polar pesticides using two-dimensional liquid chromatography high resolution mass spectrometry with electrospray ionization (ESI) and polarity switching. First results proved feasibility to determine glyphosate, AMPA, ethephon, glufosinate, MPPA, fosetyl-Al, N-acetyl-glufosinate, N-acetyl-glyphosate and N-acetyl-AMPA including fragments, next to 325 QuEChERS amenable pesticides. We plan to investigate an efficient extraction procedure by either diluting with water or acetonitrile extraction in mini scale without the need for additional clean-up steps. After completion of all experiments, the method will be validated and expanded for further pesticides and organic contaminants. Therefore, we present a concept for a Two-dimensional HILIC Reversed phase Easily Extracted Pesticides and Polar Pesticides (THREEP or 3P(+)) multi-residue method.


Assuntos
Cromatografia de Fase Reversa/métodos , Resíduos de Praguicidas/análise , Cromatografia Líquida/métodos , Interações Hidrofóbicas e Hidrofílicas , Resíduos de Praguicidas/isolamento & purificação , Espectrometria de Massas por Ionização por Electrospray
2.
Eng Life Sci ; 17(5): 479-488, 2017 May.
Artigo em Inglês | MEDLINE | ID: mdl-32624793

RESUMO

A possible application of glycerol, which is produced in large amounts as a by-product from the biodiesel industry, is its fermentation to serinol (2-amino-1,3-propanediol), a glycerol derivative. The downstream processing of this glycerol-based fermentation broth was investigated. The challenge of the isolation of serinol was the complex media and the solubility of the desired substance in aqueous media. In this study, the isolation of serinol was investigated by an appropriate reversible derivatization method. Serinol was isolated by protecting the amino group with diethyl ethoxymethylenemalonate directly in the aqueous phase, followed by extraction of the 2,2-bis(ethoxycarbonyl)vinyl-serinol (BECV-serinol) with ethyl acetate resulting in an isolated yield of 63%. We demonstrate the possibility of isolation of a hydroscopic amino alcohol from the fermentation broth and the comparison of the products in water as well as the cleavage of the 2,2-bis(ethoxycarbonyl)vinyl group (BECV group). The procedure can also be used for other amino group containing molecules, such as serine, glucosamine, hexylamine and amino methyl laureate.

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