Development of a new method using gas chromatography coupled to mass spectrometry to determine (−)-hydroxycitric acid in Garcinia gummi-gutta food supplements

Garcinia gummi-gutta based food supplements (GFS) are widely commercialized due to their antiobesity activity, which has been mainly attributed to their high content in (−)-hydroxycitric acid [(−)-HCA]. In order to overcome the limitations related to selectivity and sensitivity of the HPLC-UV method...

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Autores: Mena-García, Adal, Sanz, M. Luz, Díez-Municio, Marina, Soria, Ana C., Ruiz-Matute, Ana I.
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:2022
País:España
Institución:Consejo Superior de Investigaciones Científicas (CSIC)
Repositorio:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/280307
Acceso en línea:http://hdl.handle.net/10261/280307
Access Level:acceso abierto
Palabra clave:Garcinia gummi-gutta
Garcinia cambogia
Gas chromatography-mass spectrometry
(GC–MS)
Derivatization
Hydroxycitric acid (HCA)
Food supplements
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spelling Development of a new method using gas chromatography coupled to mass spectrometry to determine (−)-hydroxycitric acid in Garcinia gummi-gutta food supplementsMena-García, AdalSanz, M. LuzDíez-Municio, MarinaSoria, Ana C.Ruiz-Matute, Ana I.Garcinia gummi-guttaGarcinia cambogiaGas chromatography-mass spectrometry(GC–MS)DerivatizationHydroxycitric acid (HCA)Food supplementsGarcinia gummi-gutta based food supplements (GFS) are widely commercialized due to their antiobesity activity, which has been mainly attributed to their high content in (−)-hydroxycitric acid [(−)-HCA]. In order to overcome the limitations related to selectivity and sensitivity of the HPLC-UV methods usually employed for the analysis of this compound, a GC–MS method was fully developed for the first time and validated. Water with 0.1 % formic acid was used for the solubilization of (−)-HCA stabilized in the form of salt in GFS. After a drying step, different derivatization solvents were tested and only trifluoroacetic acid (TFA) allowed the complete dissolution of (−)-HCA. Regarding silylation, the best results were obtained by cold dropwise addition of hexamethyldisilazane and subsequent heating at 45 °C for 90 min. After optimizing the chromatographic conditions, the stability of derivatives for 1 month was also assessed. This new methodology was also applied to determine the (−)-HCA content of 12 commercial GFS. Experimental values ranged from 0.86 to 61%. Forty-two percent of the analyzed samples did not meet the (−)-HCA content declared on the label and 2 GFS showed HCA concentrations lower than 10% (0.86 and 6.0%), which puts into question their effectiveness in regulating obesity. One advantage of this new methodology is that it allows the qualitative and quantitative analysis of (−)-HCA in GFS without coelutions with other interfering compounds and it avoids the solubility problems presented by HCA salts. Moreover, the coupling of GC to MS provides more reliable identification of compounds present in GFS.This work is part of the I + D + I projects PID2019-106405 GB-I00 financed by MCIN/ AEI/10.13039/501100011033 and AGL2016- 80475-R, AEI/FEDER, UE, financed by MINECO. The authors would like to thank the Community of Madrid and European funding from FSE and FEDER programs for financial support (project S2018/BAA-4393, AVANSECAL-II-CM). A. Mena-García thanks the Spanish Ministry of Science, Innovation and Universities for an Industrial Doctorate grant (DIN2019-010849/AEI/10.13039/501100011033) awarded to Phar- mactive Biotech Products S.L.U.ElsevierMinisterio de Economía y Competitividad (España)European CommissionComunidad de MadridMinisterio de Ciencia e Innovación (España)Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]2022202220222022info:eu-repo/semantics/articlehttp://purl.org/coar/resource_type/c_6501Publisher's versioninfo:eu-repo/semantics/publishedVersionhttp://hdl.handle.net/10261/280307reponame:DIGITAL.CSIC. Repositorio Institucional del CSICinstname:Consejo Superior de Investigaciones Científicas (CSIC)Inglés#PLACEHOLDER_PARENT_METADATA_VALUE#info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/PID2019-106405GB-I00http://dx.doi.org/10.1016/j.microc.2022.107811Síinfo:eu-repo/semantics/openAccessoai:digital.csic.es:10261/2803072026-05-22T06:33:51Z
dc.title.none.fl_str_mv Development of a new method using gas chromatography coupled to mass spectrometry to determine (−)-hydroxycitric acid in Garcinia gummi-gutta food supplements
title Development of a new method using gas chromatography coupled to mass spectrometry to determine (−)-hydroxycitric acid in Garcinia gummi-gutta food supplements
spellingShingle Development of a new method using gas chromatography coupled to mass spectrometry to determine (−)-hydroxycitric acid in Garcinia gummi-gutta food supplements
Mena-García, Adal
Garcinia gummi-gutta
Garcinia cambogia
Gas chromatography-mass spectrometry
(GC–MS)
Derivatization
Hydroxycitric acid (HCA)
Food supplements
title_short Development of a new method using gas chromatography coupled to mass spectrometry to determine (−)-hydroxycitric acid in Garcinia gummi-gutta food supplements
title_full Development of a new method using gas chromatography coupled to mass spectrometry to determine (−)-hydroxycitric acid in Garcinia gummi-gutta food supplements
title_fullStr Development of a new method using gas chromatography coupled to mass spectrometry to determine (−)-hydroxycitric acid in Garcinia gummi-gutta food supplements
title_full_unstemmed Development of a new method using gas chromatography coupled to mass spectrometry to determine (−)-hydroxycitric acid in Garcinia gummi-gutta food supplements
title_sort Development of a new method using gas chromatography coupled to mass spectrometry to determine (−)-hydroxycitric acid in Garcinia gummi-gutta food supplements
dc.creator.none.fl_str_mv Mena-García, Adal
Sanz, M. Luz
Díez-Municio, Marina
Soria, Ana C.
Ruiz-Matute, Ana I.
author Mena-García, Adal
author_facet Mena-García, Adal
Sanz, M. Luz
Díez-Municio, Marina
Soria, Ana C.
Ruiz-Matute, Ana I.
author_role author
author2 Sanz, M. Luz
Díez-Municio, Marina
Soria, Ana C.
Ruiz-Matute, Ana I.
author2_role author
author
author
author
dc.contributor.none.fl_str_mv Ministerio de Economía y Competitividad (España)
European Commission
Comunidad de Madrid
Ministerio de Ciencia e Innovación (España)
Consejo Superior de Investigaciones Científicas [https://ror.org/02gfc7t72]
dc.subject.none.fl_str_mv Garcinia gummi-gutta
Garcinia cambogia
Gas chromatography-mass spectrometry
(GC–MS)
Derivatization
Hydroxycitric acid (HCA)
Food supplements
topic Garcinia gummi-gutta
Garcinia cambogia
Gas chromatography-mass spectrometry
(GC–MS)
Derivatization
Hydroxycitric acid (HCA)
Food supplements
description Garcinia gummi-gutta based food supplements (GFS) are widely commercialized due to their antiobesity activity, which has been mainly attributed to their high content in (−)-hydroxycitric acid [(−)-HCA]. In order to overcome the limitations related to selectivity and sensitivity of the HPLC-UV methods usually employed for the analysis of this compound, a GC–MS method was fully developed for the first time and validated. Water with 0.1 % formic acid was used for the solubilization of (−)-HCA stabilized in the form of salt in GFS. After a drying step, different derivatization solvents were tested and only trifluoroacetic acid (TFA) allowed the complete dissolution of (−)-HCA. Regarding silylation, the best results were obtained by cold dropwise addition of hexamethyldisilazane and subsequent heating at 45 °C for 90 min. After optimizing the chromatographic conditions, the stability of derivatives for 1 month was also assessed. This new methodology was also applied to determine the (−)-HCA content of 12 commercial GFS. Experimental values ranged from 0.86 to 61%. Forty-two percent of the analyzed samples did not meet the (−)-HCA content declared on the label and 2 GFS showed HCA concentrations lower than 10% (0.86 and 6.0%), which puts into question their effectiveness in regulating obesity. One advantage of this new methodology is that it allows the qualitative and quantitative analysis of (−)-HCA in GFS without coelutions with other interfering compounds and it avoids the solubility problems presented by HCA salts. Moreover, the coupling of GC to MS provides more reliable identification of compounds present in GFS.
publishDate 2022
dc.date.none.fl_str_mv 2022
2022
2022
2022
dc.type.none.fl_str_mv info:eu-repo/semantics/article
http://purl.org/coar/resource_type/c_6501
Publisher's version
info:eu-repo/semantics/publishedVersion
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/10261/280307
url http://hdl.handle.net/10261/280307
dc.language.none.fl_str_mv Inglés
language_invalid_str_mv Inglés
dc.relation.none.fl_str_mv #PLACEHOLDER_PARENT_METADATA_VALUE#
info:eu-repo/grantAgreement/AEI/Plan Estatal de Investigación Científica y Técnica y de Innovación 2017-2020/PID2019-106405GB-I00
http://dx.doi.org/10.1016/j.microc.2022.107811
Sí
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv Elsevier
publisher.none.fl_str_mv Elsevier
dc.source.none.fl_str_mv reponame:DIGITAL.CSIC. Repositorio Institucional del CSIC
instname:Consejo Superior de Investigaciones Científicas (CSIC)
instname_str Consejo Superior de Investigaciones Científicas (CSIC)
reponame_str DIGITAL.CSIC. Repositorio Institucional del CSIC
collection DIGITAL.CSIC. Repositorio Institucional del CSIC
repository.name.fl_str_mv
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