An extensive clean-up method for extraction of 17β-estradiol from eel aquaculture waste solids for quantitation via high-performance liquid chromatography tandem-mass spectrometry

Crystal L. Sweeney; Clarke A.M. Brown; Jessica L. Bennett; Neil W. Ross; Graham A. Gagnon

doi:10.1016/j.aquaculture.2021.736873

An extensive clean-up method for extraction of 17β-estradiol from eel aquaculture waste solids for quantitation via high-performance liquid chromatography tandem-mass spectrometry

Crystal L. Sweeney, Clarke A.M. Brown, Jessica L. Bennett, Neil W. Ross, Graham A. Gagnon

Medicine

Résultat de recherche: Article › examen par les pairs

1 Citation (Scopus)

Résumé

The use of 17β-estradiol (E2) in aquaculture feed increases growth and promotes feminization in freshwater eels. E2 and its metabolites (estrone (E1) and estriol (E3)) must be accurately measured in solid and liquid waste streams to ensure proper management. For reliable quantitation of estrogens in complex aquaculture waste solids, a rigorous clean-up method is imperative. The focus of this study was to assess, optimize, and validate a quick, easy, cheap, effective, rugged, and safe (QuEChERS) technique for extraction of estrogens from aquaculture waste solids and quantitation via liquid chromatography tandem-mass spectrometry (LC-MS/MS). Waste solids were collected from a recirculating aquaculture system containing American eels. Waste solids samples (2 g) were spiked to 50 μg kg⁻¹ of E1, E2, and E3 and processed using 800 mg magnesium sulfate (MgSO₄) and 400 mg of sodium acetate (NaOAc) as extraction salts. Two dispersive solid phase extraction (dSPE) steps were implemented to achieve optimal E2 recovery efficiency (RE (%)) in preliminary experiments (RE (%) = 102%; RSD = 5%). RE (%) for E1 and E3 were 87% (RSD = 54%) and 60% (RSD = 83%), respectively. Method performance characteristics were further assessed for E2 only and included specificity, linearity, accuracy (RE (%) and process efficiency (PE (%))), precision (intra-day precision, and inter-day precision), matrix effects, method detection limit (MDL), and limit of quantitation (LOQ). MDL and LOQ values for E2 were 0.7 and 2.3 μg kg⁻¹, respectively. PE (%) and RE (%) were excellent (99–101% and 99–100%, respectively) and matrix effects were minimal (99 and 101%). The results of this study indicate that this method can be used for quantitation of E2 in aquaculture waste solids.

Langue d'origine	English
Numéro d'article	736873
Journal	Aquaculture
Volume	542
DOI	https://doi.org/10.1016/j.aquaculture.2021.736873
Statut de publication	Published - sept. 15 2021

Note bibliographique

Funding Information:
The authors acknowledge funding from the Natural Science and Engineering Research Council of Canada (NSERC) (Grant # CRDPJ 537774 - 18) programs, with additional scholarship support from NSERC through the CGS-D program for Jessica L. Bennett and the USRA program for Clarke A. M. Brown. We also acknowledge NovaEel Inc. for supplying the samples used to carry out this work. We also appreciate the help and support from staff and students at the Centre for Water Resource Studies at Dalhousie University.

Funding Information:
The authors acknowledge funding from the Natural Science and Engineering Research Council of Canada (NSERC) (Grant # CRDPJ 537774 - 18 ) programs, with additional scholarship support from NSERC through the CGS-D program for Jessica L. Bennett and the USRA program for Clarke A. M. Brown. We also acknowledge NovaEel Inc. for supplying the samples used to carry out this work. We also appreciate the help and support from staff and students at the Centre for Water Resource Studies at Dalhousie University .

Publisher Copyright:
© 2021

ASJC Scopus Subject Areas

Aquatic Science

Accès au document

10.1016/j.aquaculture.2021.736873

Autres fichiers et liens

Empreinte numérique

Plonger dans les sujets de recherche 'An extensive clean-up method for extraction of 17β-estradiol from eel aquaculture waste solids for quantitation via high-performance liquid chromatography tandem-mass spectrometry'. Ensemble, ils forment une empreinte numérique unique.

Citer

@article{0bf1e44512364b4b8615cf40a18834c6,

title = "An extensive clean-up method for extraction of 17β-estradiol from eel aquaculture waste solids for quantitation via high-performance liquid chromatography tandem-mass spectrometry",

abstract = "The use of 17β-estradiol (E2) in aquaculture feed increases growth and promotes feminization in freshwater eels. E2 and its metabolites (estrone (E1) and estriol (E3)) must be accurately measured in solid and liquid waste streams to ensure proper management. For reliable quantitation of estrogens in complex aquaculture waste solids, a rigorous clean-up method is imperative. The focus of this study was to assess, optimize, and validate a quick, easy, cheap, effective, rugged, and safe (QuEChERS) technique for extraction of estrogens from aquaculture waste solids and quantitation via liquid chromatography tandem-mass spectrometry (LC-MS/MS). Waste solids were collected from a recirculating aquaculture system containing American eels. Waste solids samples (2 g) were spiked to 50 μg kg−1 of E1, E2, and E3 and processed using 800 mg magnesium sulfate (MgSO4) and 400 mg of sodium acetate (NaOAc) as extraction salts. Two dispersive solid phase extraction (dSPE) steps were implemented to achieve optimal E2 recovery efficiency (RE (%)) in preliminary experiments (RE (%) = 102%; RSD = 5%). RE (%) for E1 and E3 were 87% (RSD = 54%) and 60% (RSD = 83%), respectively. Method performance characteristics were further assessed for E2 only and included specificity, linearity, accuracy (RE (%) and process efficiency (PE (%))), precision (intra-day precision, and inter-day precision), matrix effects, method detection limit (MDL), and limit of quantitation (LOQ). MDL and LOQ values for E2 were 0.7 and 2.3 μg kg−1, respectively. PE (%) and RE (%) were excellent (99–101% and 99–100%, respectively) and matrix effects were minimal (99 and 101%). The results of this study indicate that this method can be used for quantitation of E2 in aquaculture waste solids.",

author = "Sweeney, {Crystal L.} and Brown, {Clarke A.M.} and Bennett, {Jessica L.} and Ross, {Neil W.} and Gagnon, {Graham A.}",

note = "Funding Information: The authors acknowledge funding from the Natural Science and Engineering Research Council of Canada (NSERC) (Grant # CRDPJ 537774 - 18) programs, with additional scholarship support from NSERC through the CGS-D program for Jessica L. Bennett and the USRA program for Clarke A. M. Brown. We also acknowledge NovaEel Inc. for supplying the samples used to carry out this work. We also appreciate the help and support from staff and students at the Centre for Water Resource Studies at Dalhousie University. Funding Information: The authors acknowledge funding from the Natural Science and Engineering Research Council of Canada (NSERC) (Grant # CRDPJ 537774 - 18 ) programs, with additional scholarship support from NSERC through the CGS-D program for Jessica L. Bennett and the USRA program for Clarke A. M. Brown. We also acknowledge NovaEel Inc. for supplying the samples used to carry out this work. We also appreciate the help and support from staff and students at the Centre for Water Resource Studies at Dalhousie University . Publisher Copyright: {\textcopyright} 2021",

year = "2021",

month = sep,

day = "15",

doi = "10.1016/j.aquaculture.2021.736873",

language = "English",

volume = "542",

journal = "Aquaculture",

issn = "0044-8486",

publisher = "Elsevier",

}

TY - JOUR

T1 - An extensive clean-up method for extraction of 17β-estradiol from eel aquaculture waste solids for quantitation via high-performance liquid chromatography tandem-mass spectrometry

AU - Sweeney, Crystal L.

AU - Brown, Clarke A.M.

AU - Bennett, Jessica L.

AU - Ross, Neil W.

AU - Gagnon, Graham A.

N1 - Funding Information: The authors acknowledge funding from the Natural Science and Engineering Research Council of Canada (NSERC) (Grant # CRDPJ 537774 - 18) programs, with additional scholarship support from NSERC through the CGS-D program for Jessica L. Bennett and the USRA program for Clarke A. M. Brown. We also acknowledge NovaEel Inc. for supplying the samples used to carry out this work. We also appreciate the help and support from staff and students at the Centre for Water Resource Studies at Dalhousie University. Funding Information: The authors acknowledge funding from the Natural Science and Engineering Research Council of Canada (NSERC) (Grant # CRDPJ 537774 - 18 ) programs, with additional scholarship support from NSERC through the CGS-D program for Jessica L. Bennett and the USRA program for Clarke A. M. Brown. We also acknowledge NovaEel Inc. for supplying the samples used to carry out this work. We also appreciate the help and support from staff and students at the Centre for Water Resource Studies at Dalhousie University . Publisher Copyright: © 2021

PY - 2021/9/15

Y1 - 2021/9/15

N2 - The use of 17β-estradiol (E2) in aquaculture feed increases growth and promotes feminization in freshwater eels. E2 and its metabolites (estrone (E1) and estriol (E3)) must be accurately measured in solid and liquid waste streams to ensure proper management. For reliable quantitation of estrogens in complex aquaculture waste solids, a rigorous clean-up method is imperative. The focus of this study was to assess, optimize, and validate a quick, easy, cheap, effective, rugged, and safe (QuEChERS) technique for extraction of estrogens from aquaculture waste solids and quantitation via liquid chromatography tandem-mass spectrometry (LC-MS/MS). Waste solids were collected from a recirculating aquaculture system containing American eels. Waste solids samples (2 g) were spiked to 50 μg kg−1 of E1, E2, and E3 and processed using 800 mg magnesium sulfate (MgSO4) and 400 mg of sodium acetate (NaOAc) as extraction salts. Two dispersive solid phase extraction (dSPE) steps were implemented to achieve optimal E2 recovery efficiency (RE (%)) in preliminary experiments (RE (%) = 102%; RSD = 5%). RE (%) for E1 and E3 were 87% (RSD = 54%) and 60% (RSD = 83%), respectively. Method performance characteristics were further assessed for E2 only and included specificity, linearity, accuracy (RE (%) and process efficiency (PE (%))), precision (intra-day precision, and inter-day precision), matrix effects, method detection limit (MDL), and limit of quantitation (LOQ). MDL and LOQ values for E2 were 0.7 and 2.3 μg kg−1, respectively. PE (%) and RE (%) were excellent (99–101% and 99–100%, respectively) and matrix effects were minimal (99 and 101%). The results of this study indicate that this method can be used for quantitation of E2 in aquaculture waste solids.

AB - The use of 17β-estradiol (E2) in aquaculture feed increases growth and promotes feminization in freshwater eels. E2 and its metabolites (estrone (E1) and estriol (E3)) must be accurately measured in solid and liquid waste streams to ensure proper management. For reliable quantitation of estrogens in complex aquaculture waste solids, a rigorous clean-up method is imperative. The focus of this study was to assess, optimize, and validate a quick, easy, cheap, effective, rugged, and safe (QuEChERS) technique for extraction of estrogens from aquaculture waste solids and quantitation via liquid chromatography tandem-mass spectrometry (LC-MS/MS). Waste solids were collected from a recirculating aquaculture system containing American eels. Waste solids samples (2 g) were spiked to 50 μg kg−1 of E1, E2, and E3 and processed using 800 mg magnesium sulfate (MgSO4) and 400 mg of sodium acetate (NaOAc) as extraction salts. Two dispersive solid phase extraction (dSPE) steps were implemented to achieve optimal E2 recovery efficiency (RE (%)) in preliminary experiments (RE (%) = 102%; RSD = 5%). RE (%) for E1 and E3 were 87% (RSD = 54%) and 60% (RSD = 83%), respectively. Method performance characteristics were further assessed for E2 only and included specificity, linearity, accuracy (RE (%) and process efficiency (PE (%))), precision (intra-day precision, and inter-day precision), matrix effects, method detection limit (MDL), and limit of quantitation (LOQ). MDL and LOQ values for E2 were 0.7 and 2.3 μg kg−1, respectively. PE (%) and RE (%) were excellent (99–101% and 99–100%, respectively) and matrix effects were minimal (99 and 101%). The results of this study indicate that this method can be used for quantitation of E2 in aquaculture waste solids.

UR - http://www.scopus.com/inward/record.url?scp=85105587558&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=85105587558&partnerID=8YFLogxK

U2 - 10.1016/j.aquaculture.2021.736873

DO - 10.1016/j.aquaculture.2021.736873

M3 - Article

AN - SCOPUS:85105587558

SN - 0044-8486

VL - 542

JO - Aquaculture

JF - Aquaculture

M1 - 736873

ER -