Simultaneous determination of estrogens and progestogens in honey using high performance liquid chromatography–tandem mass spectrometry
[Display omitted] •Thirteen compounds of different polarities were separated in one run.•Different washing solutions were tried to reduce impurities on solid phase extraction cartridges so as to enhance instrument sensitivity and compatibility.•The developed method could be applicable to other compl...
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Veröffentlicht in: | Journal of pharmaceutical and biomedical analysis 2016-11, Vol.131, p.303-308 |
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container_title | Journal of pharmaceutical and biomedical analysis |
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creator | Ma, Li Ashworth, Daniel Yates, Scott R. |
description | [Display omitted]
•Thirteen compounds of different polarities were separated in one run.•Different washing solutions were tried to reduce impurities on solid phase extraction cartridges so as to enhance instrument sensitivity and compatibility.•The developed method could be applicable to other complex matrices.
This work describes the development and validation of a method for the simultaneous determination of 13 estrogens and progestogens in honey by high performance liquid chromatography–tandem mass spectrometry. The hormones were preconcentrated by solid phase extraction. Pretreatment variables were optimized for a better compatibility with electrospray ionization interfaced mass spectrometry. The analytes were analyzed in multiple-reaction monitoring mode with two pairs of precursor product ion transitions. The proposed method was validated with method detection limits of 0.01–0.33ng/g and good linearities (r2>0.9901) throughout the studied concentration range. The recoveries of analytes at the spiking levels (5ng/g and 25ng/g) ranged from 71.2% to 99.7%, with relative standard deviations below 20%. The method was used to determine the target compounds in honey samples (orange blossom, clover and multiflower) obtained from supermarkets. Two samples of honey were found to contain trace amounts of estrone ( |
doi_str_mv | 10.1016/j.jpba.2016.09.001 |
format | Article |
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•Thirteen compounds of different polarities were separated in one run.•Different washing solutions were tried to reduce impurities on solid phase extraction cartridges so as to enhance instrument sensitivity and compatibility.•The developed method could be applicable to other complex matrices.
This work describes the development and validation of a method for the simultaneous determination of 13 estrogens and progestogens in honey by high performance liquid chromatography–tandem mass spectrometry. The hormones were preconcentrated by solid phase extraction. Pretreatment variables were optimized for a better compatibility with electrospray ionization interfaced mass spectrometry. The analytes were analyzed in multiple-reaction monitoring mode with two pairs of precursor product ion transitions. The proposed method was validated with method detection limits of 0.01–0.33ng/g and good linearities (r2>0.9901) throughout the studied concentration range. The recoveries of analytes at the spiking levels (5ng/g and 25ng/g) ranged from 71.2% to 99.7%, with relative standard deviations below 20%. The method was used to determine the target compounds in honey samples (orange blossom, clover and multiflower) obtained from supermarkets. Two samples of honey were found to contain trace amounts of estrone (<MQL) or progesterone (0.2±0.1ng/g), respectively.</description><identifier>ISSN: 0731-7085</identifier><identifier>EISSN: 1873-264X</identifier><identifier>DOI: 10.1016/j.jpba.2016.09.001</identifier><identifier>PMID: 27616008</identifier><language>eng</language><publisher>England: Elsevier B.V</publisher><subject>Chromatography, High Pressure Liquid - methods ; Estrogens ; Estrogens - analysis ; Estrone - analysis ; Food Contamination - analysis ; Honey - analysis ; LC–MS/MS ; Limit of Detection ; Progesterone - analysis ; Progestins - analysis ; Progestogens ; Solid phase extraction ; Solid Phase Extraction - methods ; Spectrometry, Mass, Electrospray Ionization - methods ; Tandem Mass Spectrometry - methods</subject><ispartof>Journal of pharmaceutical and biomedical analysis, 2016-11, Vol.131, p.303-308</ispartof><rights>2016</rights><rights>Published by Elsevier B.V.</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c400t-811c6d334f7d1c64d89e25bfbfa5adb707e83faf24c16d50f9ab23cd7666ec603</citedby><cites>FETCH-LOGICAL-c400t-811c6d334f7d1c64d89e25bfbfa5adb707e83faf24c16d50f9ab23cd7666ec603</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://dx.doi.org/10.1016/j.jpba.2016.09.001$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,780,784,3549,27923,27924,45994</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/27616008$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Ma, Li</creatorcontrib><creatorcontrib>Ashworth, Daniel</creatorcontrib><creatorcontrib>Yates, Scott R.</creatorcontrib><title>Simultaneous determination of estrogens and progestogens in honey using high performance liquid chromatography–tandem mass spectrometry</title><title>Journal of pharmaceutical and biomedical analysis</title><addtitle>J Pharm Biomed Anal</addtitle><description>[Display omitted]
•Thirteen compounds of different polarities were separated in one run.•Different washing solutions were tried to reduce impurities on solid phase extraction cartridges so as to enhance instrument sensitivity and compatibility.•The developed method could be applicable to other complex matrices.
This work describes the development and validation of a method for the simultaneous determination of 13 estrogens and progestogens in honey by high performance liquid chromatography–tandem mass spectrometry. The hormones were preconcentrated by solid phase extraction. Pretreatment variables were optimized for a better compatibility with electrospray ionization interfaced mass spectrometry. The analytes were analyzed in multiple-reaction monitoring mode with two pairs of precursor product ion transitions. The proposed method was validated with method detection limits of 0.01–0.33ng/g and good linearities (r2>0.9901) throughout the studied concentration range. The recoveries of analytes at the spiking levels (5ng/g and 25ng/g) ranged from 71.2% to 99.7%, with relative standard deviations below 20%. The method was used to determine the target compounds in honey samples (orange blossom, clover and multiflower) obtained from supermarkets. Two samples of honey were found to contain trace amounts of estrone (<MQL) or progesterone (0.2±0.1ng/g), respectively.</description><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Estrogens</subject><subject>Estrogens - analysis</subject><subject>Estrone - analysis</subject><subject>Food Contamination - analysis</subject><subject>Honey - analysis</subject><subject>LC–MS/MS</subject><subject>Limit of Detection</subject><subject>Progesterone - analysis</subject><subject>Progestins - analysis</subject><subject>Progestogens</subject><subject>Solid phase extraction</subject><subject>Solid Phase Extraction - methods</subject><subject>Spectrometry, Mass, Electrospray Ionization - methods</subject><subject>Tandem Mass Spectrometry - methods</subject><issn>0731-7085</issn><issn>1873-264X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2016</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNp9UbuO1TAUtBAr9rLwAxTIJU3CcR52ItGgFS9ppS0WJDrLsY9vfBUnWTtBuh0tNX-4X4KjLJRUHlkzczQzhLxikDNg_O0pP82dyouEc2hzAPaEHFgjyqzg1fen5ACiZJmApr4kz2M8AUDN2uoZuSwEZxygOZBfd86vw6JGnNZIDS4YvBvV4qaRTpZiXMJ0xDFSNRo6bzgu-4cbaT-NeKZrdOOR9u7Y0xmDnYJXo0Y6uPvVGar7MHmVNEHN_fnh5-90y6CnXsVI44w6HfC4hPMLcmHVEPHl43tFvn388PX6c3Zz--nL9fubTFcAS9Ywprkpy8oKk1BlmhaLurOdVbUynQCBTWmVLSrNuKnBtqorSm0E5xw1h_KKvNl9U5r7NcWR3kWNw7B3IFlT1qVoRbVRi52qwxRjQCvn4LwKZ8lAbhPIk9wmkNsEElqZJkii14_-a-fR_JP87TwR3u0ETCl_OAwyaoepMuNCqkOayf3P_w_MCp31</recordid><startdate>20161130</startdate><enddate>20161130</enddate><creator>Ma, Li</creator><creator>Ashworth, Daniel</creator><creator>Yates, Scott R.</creator><general>Elsevier B.V</general><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7X8</scope></search><sort><creationdate>20161130</creationdate><title>Simultaneous determination of estrogens and progestogens in honey using high performance liquid chromatography–tandem mass spectrometry</title><author>Ma, Li ; Ashworth, Daniel ; Yates, Scott R.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c400t-811c6d334f7d1c64d89e25bfbfa5adb707e83faf24c16d50f9ab23cd7666ec603</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2016</creationdate><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Estrogens</topic><topic>Estrogens - analysis</topic><topic>Estrone - analysis</topic><topic>Food Contamination - analysis</topic><topic>Honey - analysis</topic><topic>LC–MS/MS</topic><topic>Limit of Detection</topic><topic>Progesterone - analysis</topic><topic>Progestins - analysis</topic><topic>Progestogens</topic><topic>Solid phase extraction</topic><topic>Solid Phase Extraction - methods</topic><topic>Spectrometry, Mass, Electrospray Ionization - methods</topic><topic>Tandem Mass Spectrometry - methods</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Ma, Li</creatorcontrib><creatorcontrib>Ashworth, Daniel</creatorcontrib><creatorcontrib>Yates, Scott R.</creatorcontrib><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><jtitle>Journal of pharmaceutical and biomedical analysis</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Ma, Li</au><au>Ashworth, Daniel</au><au>Yates, Scott R.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Simultaneous determination of estrogens and progestogens in honey using high performance liquid chromatography–tandem mass spectrometry</atitle><jtitle>Journal of pharmaceutical and biomedical analysis</jtitle><addtitle>J Pharm Biomed Anal</addtitle><date>2016-11-30</date><risdate>2016</risdate><volume>131</volume><spage>303</spage><epage>308</epage><pages>303-308</pages><issn>0731-7085</issn><eissn>1873-264X</eissn><abstract>[Display omitted]
•Thirteen compounds of different polarities were separated in one run.•Different washing solutions were tried to reduce impurities on solid phase extraction cartridges so as to enhance instrument sensitivity and compatibility.•The developed method could be applicable to other complex matrices.
This work describes the development and validation of a method for the simultaneous determination of 13 estrogens and progestogens in honey by high performance liquid chromatography–tandem mass spectrometry. The hormones were preconcentrated by solid phase extraction. Pretreatment variables were optimized for a better compatibility with electrospray ionization interfaced mass spectrometry. The analytes were analyzed in multiple-reaction monitoring mode with two pairs of precursor product ion transitions. The proposed method was validated with method detection limits of 0.01–0.33ng/g and good linearities (r2>0.9901) throughout the studied concentration range. The recoveries of analytes at the spiking levels (5ng/g and 25ng/g) ranged from 71.2% to 99.7%, with relative standard deviations below 20%. The method was used to determine the target compounds in honey samples (orange blossom, clover and multiflower) obtained from supermarkets. Two samples of honey were found to contain trace amounts of estrone (<MQL) or progesterone (0.2±0.1ng/g), respectively.</abstract><cop>England</cop><pub>Elsevier B.V</pub><pmid>27616008</pmid><doi>10.1016/j.jpba.2016.09.001</doi><tpages>6</tpages><oa>free_for_read</oa></addata></record> |
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subjects | Chromatography, High Pressure Liquid - methods Estrogens Estrogens - analysis Estrone - analysis Food Contamination - analysis Honey - analysis LC–MS/MS Limit of Detection Progesterone - analysis Progestins - analysis Progestogens Solid phase extraction Solid Phase Extraction - methods Spectrometry, Mass, Electrospray Ionization - methods Tandem Mass Spectrometry - methods |
title | Simultaneous determination of estrogens and progestogens in honey using high performance liquid chromatography–tandem mass spectrometry |
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