Development and validation of a method for simultaneous analysis of the boar taint compounds indole, skatole and androstenone in pig fat using liquid chromatography–multiple mass spectrometry
Boar taint in entire male pigs remains a problem for fresh pork production. Since castration of pigs will be prohibited in the future on animal welfare reasons, attempts are made to detect boar taint pre and post mortem. Post mortem techniques focus on simultaneous quantification of the three boar t...
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Published in | Journal of Chromatography A Vol. 1174; no. 1; pp. 132 - 137 |
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Main Authors | , , , , , |
Format | Journal Article Conference Proceeding |
Language | English |
Published |
Amsterdam
Elsevier B.V
07.12.2007
Elsevier |
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Abstract | Boar taint in entire male pigs remains a problem for fresh pork production. Since castration of pigs will be prohibited in the future on animal welfare reasons, attempts are made to detect boar taint pre and post mortem. Post mortem techniques focus on simultaneous quantification of the three boar taint substances by one simple and reliable method. In this study a liquid chromatographic multiple mass spectrometric (LC–MS
n
) method has been developed and validated for the simultaneous determination of indole (2,3-benzopyrrole, ID), skatole (3-methylindole, SK) and androstenone (5α-androst-16-en-3-one, AEON) in pig fat samples. Sample preparation was kept as short as possible, since a single extraction method for structurally different indols and steroids was seeked after. Analytes were extracted from the fat matrix by methanol and clean-up consisted of freezing the extract in liquid nitrogen followed by a filtration step. The analytes were chromatographically separated on a Symmetry C
18 column. Recoveries for ID, SK and AEON, as calculated from fortified fat samples using 2-methylindole (2-MID) as internal standard, were 96, 91 and 104%, respectively. However, matrix interferences were encountered determining the androstenone levels in fat. Linearity, determined in fat samples, was in the range of 50–1600
μg
kg
−1 for the indolic compounds and 125–2000
μg
kg
−1 for the steroid AEON. The correlation coefficients (
R
2) of the calibration curves were 0.998 for ID, 0.997 for SK and 0.810 for AEON. |
---|---|
AbstractList | Boar taint in entire male pigs remains a problem for fresh pork production. Since castration of pigs will be prohibited in the future on animal welfare reasons, attempts are made to detect boar taint pre and post mortem. Post mortem techniques focus on simultaneous quantification of the three boar taint substances by one simple and reliable method. In this study a liquid chromatographic multiple mass spectrometric (LC–MS
n
) method has been developed and validated for the simultaneous determination of indole (2,3-benzopyrrole, ID), skatole (3-methylindole, SK) and androstenone (5α-androst-16-en-3-one, AEON) in pig fat samples. Sample preparation was kept as short as possible, since a single extraction method for structurally different indols and steroids was seeked after. Analytes were extracted from the fat matrix by methanol and clean-up consisted of freezing the extract in liquid nitrogen followed by a filtration step. The analytes were chromatographically separated on a Symmetry C
18 column. Recoveries for ID, SK and AEON, as calculated from fortified fat samples using 2-methylindole (2-MID) as internal standard, were 96, 91 and 104%, respectively. However, matrix interferences were encountered determining the androstenone levels in fat. Linearity, determined in fat samples, was in the range of 50–1600
μg
kg
−1 for the indolic compounds and 125–2000
μg
kg
−1 for the steroid AEON. The correlation coefficients (
R
2) of the calibration curves were 0.998 for ID, 0.997 for SK and 0.810 for AEON. Boar taint in entire male pigs remains a problem for fresh pork production. Since castration of pigs will be prohibited in the future on animal welfare reasons, attempts are made to detect boar taint pre and post mortem. Post mortem techniques focus on simultaneous quantification of the three boar taint substances by one simple and reliable method. In this study a liquid chromatographic multiple mass spectrometric (LC-MS(n)) method has been developed and validated for the simultaneous determination of indole (2,3-benzopyrrole, ID), skatole (3-methylindole, SK) and androstenone (5alpha-androst-16-en-3-one, AEON) in pig fat samples. Sample preparation was kept as short as possible, since a single extraction method for structurally different indols and steroids was seeked after. Analytes were extracted from the fat matrix by methanol and clean-up consisted of freezing the extract in liquid nitrogen followed by a filtration step. The analytes were chromatographically separated on a Symmetry C(18) column. Recoveries for ID, SK and AEON, as calculated from fortified fat samples using 2-methylindole (2-MID) as internal standard, were 96, 91 and 104%, respectively. However, matrix interferences were encountered determining the androstenone levels in fat. Linearity, determined in fat samples, was in the range of 50-1600 microg kg(-1) for the indolic compounds and 125-2000 microg kg(-1) for the steroid AEON. The correlation coefficients (R(2)) of the calibration curves were 0.998 for ID, 0.997 for SK and 0.810 for AEON. |
Author | Aluwé, M. De Brabander, H.F. Verheyden, K. Millet, S. Vanden Bussche, J. Noppe, H. |
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Keywords | Fat matrix Skatole Androstenone Indole LC–MS n Boar taint Steroid Tandem mass spectrometry Chemical analysis Atmospheric pressure LC-MSn Solvent extraction Electrospray Off-flavor Sample preparation Ungulata Quantitative analysis Validation Filtration Coupled method Chemical ionization Pig Vertebrata Reversed phase chromatography Mammalia Simultaneous measurement Fat Artiodactyla Indole derivatives |
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Snippet | Boar taint in entire male pigs remains a problem for fresh pork production. Since castration of pigs will be prohibited in the future on animal welfare... |
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SubjectTerms | Analytical chemistry Androstenes - analysis Androstenone Animals Biological and medical sciences Boar taint body fat Calibration chemical analysis Chemistry Chromatographic methods and physical methods associated with chromatography Chromatography, Liquid - methods Exact sciences and technology Fat matrix food analysis Food industries Fundamental and applied biological sciences. Psychology Indole indoles Indoles - analysis lard LC–MS n Lipids - chemistry liquid chromatography mass spectrometry Mass Spectrometry - methods Meat and meat product industries Other chromatographic methods pork Reproducibility of Results Skatole Skatole - analysis swine Swine - metabolism |
Title | Development and validation of a method for simultaneous analysis of the boar taint compounds indole, skatole and androstenone in pig fat using liquid chromatography–multiple mass spectrometry |
URI | https://dx.doi.org/10.1016/j.chroma.2007.08.075 https://www.ncbi.nlm.nih.gov/pubmed/17889887 https://search.proquest.com/docview/68546475 |
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