Rapid Determination of Illegally Added 25 Hormones in Oral by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
Xiaoqi He
Abstract
Xiaoqi He
Abstract
A sensitive ultra performance liquid chromatography-tandem mass spectrometric( UPLC-MS /MS) method was developed for the simultaneous determination of 9 progesterones,7 androgens,7 glucocorticoids,2 estrogens in anti-aging oral samples. The analytes were stepwise extracted with acetonitrile containing 1% acetic acid and methanol,the extract was concentrated to dryness,redissolved in methanol-water( 1 ∶ 1). 25 hormones were gradient separated on a Shim-pack XR-ODS Ⅱ column,and analyzed by electrospray ionization under positive ion mode with matrix standard curve. As a result,the calibration curves for all target compounds were linear in the range of 0. 5-50 μg /L with correlation coefficients larger than 0. 99. The limits of detection( LOD) ranged from0. 029 μg /kg to 0. 147 μg /kg and the limits of quantitation( LOQ) ranged from 0. 099 μg /kg to0. 492 μg /kg. The average recoveries of 25 compounds at spiked levels of 0. 5,1. 0,5. 0 μg /kg were in the range of 73. 3%-122. 2% with relative standard deviations( RSD) of 5. 1%-14. 9%.The method is simple,rapid and accurate,and is suitable for the rapid determination of hormones in anti-aging function foods.
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A sensitive ultra performance liquid chromatography-tandem mass spectrometric( UPLC-MS /MS) method was developed for the simultaneous determination of 9 progesterones,7 androgens,7 glucocorticoids,2 estrogens in anti-aging oral samples. The analytes were stepwise extracted with acetonitrile containing 1% acetic acid and methanol,the extract was concentrated to dryness,redissolved in methanol-water( 1 ∶ 1). 25 hormones were gradient separated on a Shim-pack XR-ODS Ⅱ column,and analyzed by electrospray ionization under positive ion mode with matrix standard curve. As a result,the calibration curves for all target compounds were linear in the range of 0. 5-50 μg /L with correlation coefficients larger than 0. 99. The limits of detection( LOD) ranged from0. 029 μg /kg to 0. 147 μg /kg and the limits of quantitation( LOQ) ranged from 0. 099 μg /kg to0. 492 μg /kg. The average recoveries of 25 compounds at spiked levels of 0. 5,1. 0,5. 0 μg /kg were in the range of 73. 3%-122. 2% with relative standard deviations( RSD) of 5. 1%-14. 9%.The method is simple,rapid and accurate,and is suitable for the rapid determination of hormones in anti-aging function foods.
Key concepts: Chemistry, Chromatography, Detection limit, Calibration curve, Electrospray ionization, Tandem mass spectrometry, Mass spectrometry, Selected reaction monitoring