Development of an RP-UHPLC-PDA method for quantification of free gossypol in cottonseed cake and fungal-treated cottonseed cake.

Cottonseed cake biomass, which is a residue of oil extraction, is potentially appropriate for use as animal feed, given the high mineral, fibre and protein content. The presence of free gossypol, however, a toxic pigment in the glands of the cotton plant, limits use of this biomass for monogastric l...

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Main Authors: Aparecido Almeida Conceição, Clemente Batista Soares Neto, José Antônio de Aquino Ribeiro, Felix Gonçalves de Siqueira, Robert Neil Gerard Miller, Simone Mendonça
Format: Article
Language:English
Published: Public Library of Science (PLoS) 2018-01-01
Series:PLoS ONE
Online Access:http://europepmc.org/articles/PMC5965856?pdf=render
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author Aparecido Almeida Conceição
Clemente Batista Soares Neto
José Antônio de Aquino Ribeiro
Felix Gonçalves de Siqueira
Robert Neil Gerard Miller
Simone Mendonça
author_facet Aparecido Almeida Conceição
Clemente Batista Soares Neto
José Antônio de Aquino Ribeiro
Felix Gonçalves de Siqueira
Robert Neil Gerard Miller
Simone Mendonça
author_sort Aparecido Almeida Conceição
collection DOAJ
description Cottonseed cake biomass, which is a residue of oil extraction, is potentially appropriate for use as animal feed, given the high mineral, fibre and protein content. The presence of free gossypol, however, a toxic pigment in the glands of the cotton plant, limits use of this biomass for monogastric livestock. A promising method to detoxify cottonseed cake relies on fermentation by fungi, which can eliminate up to 100% of gossypol. In order to quantify trace levels of free gossypol in different cotton materials, including cottonseed cake treated with macrofungi, a simple and rapid chromatographic detection method was developed and validated. Under optimized conditions, extraction was performed using 70% acetone. The extract was then analysed by Ultra High-Performance Liquid Chromatography (UHPLC), with gradient elution on a C18 reverse phase column KINETEX® (100 x 2.10 mm, 2.6 μm). Methanol-0.1% TFA aqueous solution was employed as mobile phase and PDA detection conducted at 254 nm. The optimized method was validated by analysis of specificity, linearity and range, limit of detection, limit of quantification, precision and accuracy. Detection and quantification limits were observed at 0.2 and 0.5 μg/mL, respectively. With good reproducibility, with precision (RSD)<10% and recovery greater than 94%, the developed assay was appropriate for quantification of low quantities of free gossypol. The validated method was successfully applied to determine trace levels of free gossypol cottonseed treated with a macrofungus.
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spelling doaj.art-092f3ee64e6d4e118d8fde448d0d14972022-12-22T02:37:29ZengPublic Library of Science (PLoS)PLoS ONE1932-62032018-01-01135e019616410.1371/journal.pone.0196164Development of an RP-UHPLC-PDA method for quantification of free gossypol in cottonseed cake and fungal-treated cottonseed cake.Aparecido Almeida ConceiçãoClemente Batista Soares NetoJosé Antônio de Aquino RibeiroFelix Gonçalves de SiqueiraRobert Neil Gerard MillerSimone MendonçaCottonseed cake biomass, which is a residue of oil extraction, is potentially appropriate for use as animal feed, given the high mineral, fibre and protein content. The presence of free gossypol, however, a toxic pigment in the glands of the cotton plant, limits use of this biomass for monogastric livestock. A promising method to detoxify cottonseed cake relies on fermentation by fungi, which can eliminate up to 100% of gossypol. In order to quantify trace levels of free gossypol in different cotton materials, including cottonseed cake treated with macrofungi, a simple and rapid chromatographic detection method was developed and validated. Under optimized conditions, extraction was performed using 70% acetone. The extract was then analysed by Ultra High-Performance Liquid Chromatography (UHPLC), with gradient elution on a C18 reverse phase column KINETEX® (100 x 2.10 mm, 2.6 μm). Methanol-0.1% TFA aqueous solution was employed as mobile phase and PDA detection conducted at 254 nm. The optimized method was validated by analysis of specificity, linearity and range, limit of detection, limit of quantification, precision and accuracy. Detection and quantification limits were observed at 0.2 and 0.5 μg/mL, respectively. With good reproducibility, with precision (RSD)<10% and recovery greater than 94%, the developed assay was appropriate for quantification of low quantities of free gossypol. The validated method was successfully applied to determine trace levels of free gossypol cottonseed treated with a macrofungus.http://europepmc.org/articles/PMC5965856?pdf=render
spellingShingle Aparecido Almeida Conceição
Clemente Batista Soares Neto
José Antônio de Aquino Ribeiro
Felix Gonçalves de Siqueira
Robert Neil Gerard Miller
Simone Mendonça
Development of an RP-UHPLC-PDA method for quantification of free gossypol in cottonseed cake and fungal-treated cottonseed cake.
PLoS ONE
title Development of an RP-UHPLC-PDA method for quantification of free gossypol in cottonseed cake and fungal-treated cottonseed cake.
title_full Development of an RP-UHPLC-PDA method for quantification of free gossypol in cottonseed cake and fungal-treated cottonseed cake.
title_fullStr Development of an RP-UHPLC-PDA method for quantification of free gossypol in cottonseed cake and fungal-treated cottonseed cake.
title_full_unstemmed Development of an RP-UHPLC-PDA method for quantification of free gossypol in cottonseed cake and fungal-treated cottonseed cake.
title_short Development of an RP-UHPLC-PDA method for quantification of free gossypol in cottonseed cake and fungal-treated cottonseed cake.
title_sort development of an rp uhplc pda method for quantification of free gossypol in cottonseed cake and fungal treated cottonseed cake
url http://europepmc.org/articles/PMC5965856?pdf=render
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