Determination of estrogenic compounds in milk and yogurt samples by hollow-fibre liquid-phase microextraction-gas chromatography-triple quadrupole mass spectrometry
An environmentally friendly method based on hollow-fibre liquid-phase microextraction (HF-LPME) was developed for the extraction of selected estrogenic compounds (i.e. four natural sexual hormones: estrone, 17β-estradiol, 17α-estradiol and estriol; two exoestrogens: 17α-ethynylestradiol and 2-methox...
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| Veröffentlicht in: | Analytical and bioanalytical chemistry 2016-10, Vol.408 (26), p.7447-7459 |
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| creator | D’Orazio, Giovanni Hernández-Borges, Javier Herrera-Herrera, Antonio Vicente Fanali, Salvatore Rodríguez-Delgado, Miguel Ángel |
| description | An environmentally friendly method based on hollow-fibre liquid-phase microextraction (HF-LPME) was developed for the extraction of selected estrogenic compounds (i.e. four natural sexual hormones: estrone, 17β-estradiol, 17α-estradiol and estriol; two exoestrogens: 17α-ethynylestradiol and 2-methoxyestradiol; two synthetic stilbenes: dienestrol and hexestrol; and five resorcylic acid lactones: zearalenone, α-zearalanol, β-zearalanol, α-zearalenol and β-zearalenol), from whole cow and semi-skimmed goat milk and whole natural yogurt. After the optimization of the sample preparation procedure, spiked extracts were derivatized to their trimethylsilyl products using
N
,
O
-bis(trimethylsilyl)trifluoroacetamide reagent and then analyzed by gas chromatography–tandem mass spectrometry (GC-MS/MS). Once optimum extraction conditions were established (protein precipitation with acetonitrile, extraction and the back-extraction in acetonitrile following the HF-LPME procedure), the method was validated and the calibration range, precision and accuracy were studied. The RSD values for the intra- and inter-day precision of the peak areas were in the range 0.65–9.69 and 1.00–11.47 %, respectively. The determination coefficients were higher than 0.991 for method calibration curves while LOD and LOQ values were between 0.06–2.55 and 0.16–6.11 μg/L for whole cow milk, 0.04–1.70 and 0.11–4.86 μg/L for semi-skimmed goat milk and 0.07–3.73 and 0.23–9.81 μg/L for natural yogurt, respectively. Finally, the accuracy and precision of the method were evaluated, obtaining a value in the range 84 81–119 % and RSD values lower than 20 % in all cases. |
| doi_str_mv | 10.1007/s00216-016-9833-0 |
| format | Article |
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N
,
O
-bis(trimethylsilyl)trifluoroacetamide reagent and then analyzed by gas chromatography–tandem mass spectrometry (GC-MS/MS). Once optimum extraction conditions were established (protein precipitation with acetonitrile, extraction and the back-extraction in acetonitrile following the HF-LPME procedure), the method was validated and the calibration range, precision and accuracy were studied. The RSD values for the intra- and inter-day precision of the peak areas were in the range 0.65–9.69 and 1.00–11.47 %, respectively. The determination coefficients were higher than 0.991 for method calibration curves while LOD and LOQ values were between 0.06–2.55 and 0.16–6.11 μg/L for whole cow milk, 0.04–1.70 and 0.11–4.86 μg/L for semi-skimmed goat milk and 0.07–3.73 and 0.23–9.81 μg/L for natural yogurt, respectively. Finally, the accuracy and precision of the method were evaluated, obtaining a value in the range 84 81–119 % and RSD values lower than 20 % in all cases.</description><identifier>ISSN: 1618-2642</identifier><identifier>EISSN: 1618-2650</identifier><identifier>DOI: 10.1007/s00216-016-9833-0</identifier><identifier>PMID: 27526090</identifier><language>eng</language><publisher>Berlin/Heidelberg: Springer Berlin Heidelberg</publisher><subject>Acetonitrile ; Analytical Chemistry ; Animals ; Biochemistry ; Calibration ; Cattle ; Characterization and Evaluation of Materials ; Chemical properties ; Chemistry ; Chemistry and Materials Science ; Chromatography ; Contamination ; Dairy products ; Estrogens ; Estrogens - analysis ; Estrogens - isolation & purification ; Extraction ; Extraction (Chemistry) ; Food ; Food Analysis - methods ; Food Contamination - analysis ; Food Science ; Food testing ; Gas chromatography ; Gas Chromatography-Mass Spectrometry - methods ; Goats ; Hormones ; Laboratory Medicine ; Limit of Detection ; Liquid Phase Microextraction - methods ; Mass spectrometry ; Metabolites ; Methods ; Milk ; Milk - chemistry ; Monitoring/Environmental Analysis ; Optimization ; Reagents ; Research Paper ; Sample preparation ; Scientific imaging ; Yogurt ; Yogurt - analysis</subject><ispartof>Analytical and bioanalytical chemistry, 2016-10, Vol.408 (26), p.7447-7459</ispartof><rights>Springer-Verlag Berlin Heidelberg 2016</rights><rights>COPYRIGHT 2016 Springer</rights><rights>Analytical and Bioanalytical Chemistry is a copyright of Springer, 2016.</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c542t-f5901fa3c1281d53034d8a1a1a6b1c1699fc7e958a499d636d65db22fd9d28c3</citedby><cites>FETCH-LOGICAL-c542t-f5901fa3c1281d53034d8a1a1a6b1c1699fc7e958a499d636d65db22fd9d28c3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://link.springer.com/content/pdf/10.1007/s00216-016-9833-0$$EPDF$$P50$$Gspringer$$H</linktopdf><linktohtml>$$Uhttps://link.springer.com/10.1007/s00216-016-9833-0$$EHTML$$P50$$Gspringer$$H</linktohtml><link.rule.ids>314,780,784,27922,27923,41486,42555,51317</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/27526090$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>D’Orazio, Giovanni</creatorcontrib><creatorcontrib>Hernández-Borges, Javier</creatorcontrib><creatorcontrib>Herrera-Herrera, Antonio Vicente</creatorcontrib><creatorcontrib>Fanali, Salvatore</creatorcontrib><creatorcontrib>Rodríguez-Delgado, Miguel Ángel</creatorcontrib><title>Determination of estrogenic compounds in milk and yogurt samples by hollow-fibre liquid-phase microextraction-gas chromatography-triple quadrupole mass spectrometry</title><title>Analytical and bioanalytical chemistry</title><addtitle>Anal Bioanal Chem</addtitle><addtitle>Anal Bioanal Chem</addtitle><description>An environmentally friendly method based on hollow-fibre liquid-phase microextraction (HF-LPME) was developed for the extraction of selected estrogenic compounds (i.e. four natural sexual hormones: estrone, 17β-estradiol, 17α-estradiol and estriol; two exoestrogens: 17α-ethynylestradiol and 2-methoxyestradiol; two synthetic stilbenes: dienestrol and hexestrol; and five resorcylic acid lactones: zearalenone, α-zearalanol, β-zearalanol, α-zearalenol and β-zearalenol), from whole cow and semi-skimmed goat milk and whole natural yogurt. After the optimization of the sample preparation procedure, spiked extracts were derivatized to their trimethylsilyl products using
N
,
O
-bis(trimethylsilyl)trifluoroacetamide reagent and then analyzed by gas chromatography–tandem mass spectrometry (GC-MS/MS). Once optimum extraction conditions were established (protein precipitation with acetonitrile, extraction and the back-extraction in acetonitrile following the HF-LPME procedure), the method was validated and the calibration range, precision and accuracy were studied. The RSD values for the intra- and inter-day precision of the peak areas were in the range 0.65–9.69 and 1.00–11.47 %, respectively. The determination coefficients were higher than 0.991 for method calibration curves while LOD and LOQ values were between 0.06–2.55 and 0.16–6.11 μg/L for whole cow milk, 0.04–1.70 and 0.11–4.86 μg/L for semi-skimmed goat milk and 0.07–3.73 and 0.23–9.81 μg/L for natural yogurt, respectively. Finally, the accuracy and precision of the method were evaluated, obtaining a value in the range 84 81–119 % and RSD values lower than 20 % in all cases.</description><subject>Acetonitrile</subject><subject>Analytical Chemistry</subject><subject>Animals</subject><subject>Biochemistry</subject><subject>Calibration</subject><subject>Cattle</subject><subject>Characterization and Evaluation of Materials</subject><subject>Chemical properties</subject><subject>Chemistry</subject><subject>Chemistry and Materials Science</subject><subject>Chromatography</subject><subject>Contamination</subject><subject>Dairy products</subject><subject>Estrogens</subject><subject>Estrogens - analysis</subject><subject>Estrogens - isolation & purification</subject><subject>Extraction</subject><subject>Extraction (Chemistry)</subject><subject>Food</subject><subject>Food Analysis - methods</subject><subject>Food Contamination - analysis</subject><subject>Food Science</subject><subject>Food testing</subject><subject>Gas chromatography</subject><subject>Gas Chromatography-Mass Spectrometry - methods</subject><subject>Goats</subject><subject>Hormones</subject><subject>Laboratory Medicine</subject><subject>Limit of Detection</subject><subject>Liquid Phase Microextraction - methods</subject><subject>Mass spectrometry</subject><subject>Metabolites</subject><subject>Methods</subject><subject>Milk</subject><subject>Milk - chemistry</subject><subject>Monitoring/Environmental Analysis</subject><subject>Optimization</subject><subject>Reagents</subject><subject>Research Paper</subject><subject>Sample preparation</subject><subject>Scientific imaging</subject><subject>Yogurt</subject><subject>Yogurt - 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of estrogenic compounds in milk and yogurt samples by hollow-fibre liquid-phase microextraction-gas chromatography-triple quadrupole mass spectrometry</title><author>D’Orazio, Giovanni ; Hernández-Borges, Javier ; Herrera-Herrera, Antonio Vicente ; Fanali, Salvatore ; Rodríguez-Delgado, Miguel Ángel</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c542t-f5901fa3c1281d53034d8a1a1a6b1c1699fc7e958a499d636d65db22fd9d28c3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2016</creationdate><topic>Acetonitrile</topic><topic>Analytical Chemistry</topic><topic>Animals</topic><topic>Biochemistry</topic><topic>Calibration</topic><topic>Cattle</topic><topic>Characterization and Evaluation of Materials</topic><topic>Chemical properties</topic><topic>Chemistry</topic><topic>Chemistry and Materials Science</topic><topic>Chromatography</topic><topic>Contamination</topic><topic>Dairy 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Chem</addtitle><date>2016-10-01</date><risdate>2016</risdate><volume>408</volume><issue>26</issue><spage>7447</spage><epage>7459</epage><pages>7447-7459</pages><issn>1618-2642</issn><eissn>1618-2650</eissn><abstract>An environmentally friendly method based on hollow-fibre liquid-phase microextraction (HF-LPME) was developed for the extraction of selected estrogenic compounds (i.e. four natural sexual hormones: estrone, 17β-estradiol, 17α-estradiol and estriol; two exoestrogens: 17α-ethynylestradiol and 2-methoxyestradiol; two synthetic stilbenes: dienestrol and hexestrol; and five resorcylic acid lactones: zearalenone, α-zearalanol, β-zearalanol, α-zearalenol and β-zearalenol), from whole cow and semi-skimmed goat milk and whole natural yogurt. After the optimization of the sample preparation procedure, spiked extracts were derivatized to their trimethylsilyl products using
N
,
O
-bis(trimethylsilyl)trifluoroacetamide reagent and then analyzed by gas chromatography–tandem mass spectrometry (GC-MS/MS). Once optimum extraction conditions were established (protein precipitation with acetonitrile, extraction and the back-extraction in acetonitrile following the HF-LPME procedure), the method was validated and the calibration range, precision and accuracy were studied. The RSD values for the intra- and inter-day precision of the peak areas were in the range 0.65–9.69 and 1.00–11.47 %, respectively. The determination coefficients were higher than 0.991 for method calibration curves while LOD and LOQ values were between 0.06–2.55 and 0.16–6.11 μg/L for whole cow milk, 0.04–1.70 and 0.11–4.86 μg/L for semi-skimmed goat milk and 0.07–3.73 and 0.23–9.81 μg/L for natural yogurt, respectively. Finally, the accuracy and precision of the method were evaluated, obtaining a value in the range 84 81–119 % and RSD values lower than 20 % in all cases.</abstract><cop>Berlin/Heidelberg</cop><pub>Springer Berlin Heidelberg</pub><pmid>27526090</pmid><doi>10.1007/s00216-016-9833-0</doi><tpages>13</tpages></addata></record> |
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| subjects | Acetonitrile Analytical Chemistry Animals Biochemistry Calibration Cattle Characterization and Evaluation of Materials Chemical properties Chemistry Chemistry and Materials Science Chromatography Contamination Dairy products Estrogens Estrogens - analysis Estrogens - isolation & purification Extraction Extraction (Chemistry) Food Food Analysis - methods Food Contamination - analysis Food Science Food testing Gas chromatography Gas Chromatography-Mass Spectrometry - methods Goats Hormones Laboratory Medicine Limit of Detection Liquid Phase Microextraction - methods Mass spectrometry Metabolites Methods Milk Milk - chemistry Monitoring/Environmental Analysis Optimization Reagents Research Paper Sample preparation Scientific imaging Yogurt Yogurt - analysis |
| title | Determination of estrogenic compounds in milk and yogurt samples by hollow-fibre liquid-phase microextraction-gas chromatography-triple quadrupole mass spectrometry |
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