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Determination of 12 Kinds of Estrogenic and Progesterone Hormones in Infant Formula Milk Powder by Ultra Fast Liquid Chromatography-Ion Trap-Time of Flight Mass Spectrometry |
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DOI:10.3969/j.issn.1004-4957.年份.月份 |
KeyWord:ultra fast liquid chromatography-ion trap-time of flight mass spectrometry(UFLC-IT-TOF-MS) estrogenic and progesterone hormones infant formula milk powder |
Author | Institution |
张晓波,黄丽英,陈小珍,曹慧,武晓光,祝颖,莫卫民 |
1.浙江工业大学化学工程与材料学院;2.浙江省质量检测科学研究院 |
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Abstract: |
A method was developed for the determination of 12 kinds of estrogenic and progesterone hormones in infant formula milk powder using ultra fast liquid chromatography-ion trap-time of flight mass spectrometry(UFLC-IT-TOF-MS).The milk powder was dissolved in warm water,and extracted with ethyl acetate after enzymatic hydrolysis.The extract was cleaned up on an HLB cartridge.The estrogenic and progesterone hormones were separated on Shim pack XR-ODSⅡand HSS T3 columns,and then analyzed in ESI- mode for estrogens and ESI+ mode for progesterones.The calibration curves of the target compounds were linear in the range of 1.0-200 μg/L with correlation coefficients greater than 0.998.The average spiked recoveries were in the range of 79.9%-110.4% with relative standard deviations of 2.8%-8.0%.The limits of detection(LODs) ranged from 0.3 μg/kg to 0.6 μg/kg and the limits of quantitation(LOQ) ranged from 0.9 μg/kg to 1.8 μg/kg.The mass errors between theoretical and experimental masses were obtained for deprotonated molecule of 12 estrogenic and progesterone hormones,and the main possible fragmentation pathway of estrone was verified. |
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