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
Hauptverfasser: Ma, Li, Ashworth, Daniel, Yates, Scott R.
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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 (
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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&gt;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. 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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&gt;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. 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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&gt;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. 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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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