Study On The Estrogenic And Progesterone Hormones Residues In Animal-derived Food By Liquid Chromatography And Mass Spectrometry

The analysis and detection of estrogenic and progesterone hormones residues in animal-derived food is an important aspect of food safety regulation,but also a focus of people concerned about food safety Hormone drug residues enter the human body through the food chain,not only seriously affect the normal physiological functions of the human body,,and some exogenous hormones also have mutagenic,teratogenic,carcinogenic potential hazards.The analysis and detection of estrogen and progesterone residues in food,for the protection of consumers' health and ensuring food safety is important.The screening and determination methods for estrogenic and progesterone hormones in infant formula milk powder,eggs and duck meat were established respectively using LCMS-IT-TOF?LC-MS/MS.It includes five chapters as follows:(1)The common knowledge of estrogenic and progesterone hormones were summarized briefly.Besides,the research status of analysis methods in recent years and the sample pretreatment technique were reviewed.(2)A method for the determination of 12 kinds of estrogenic and progesterone hormones in infant formula.The milk powder was dissolved in appropriate water,and extracted with acetonitrile after enzymatic hydrolysis.The extract solution was cleaned up on an HLB.The estrogenic and progesterone hormones were separated on Shim-pack XR-ODS ? and HSS T3 columns,and then analyzed in ESI-mode for estrogens and ESI+mode for progesterones.The result indicate that using the LCMS-IT-TOF and UPLC-MS/MS methods,12 kinds of estrogenic and progesterone hormones showed good linearities in the range of 1.0?100.0 ?g/L and high correlation coefficents(r~2>0.99).The detction limits were in the range of 0.2?0.6 ?g/kg and the quantitation limits were in the range of 0.6?1.5?g/kg.The mean recoveries at three spiked level ranged from 77.9%?110.4%by LCMS-IT-TOF method,and ranged from 80.2%?108.7%by UPLC-MS/MS method.(3)A method for the determination of 4 kinds of progesterone hormones in egg by DSPE as clean up step and mass spectrometry as detection step.Residues were extracted by n-hexane with PSA dispersive solid-phase extraction clean up.The targeted compounds were separated on a column and quantified by the matrix matched external standard method except for progesterone.The result indicate that using the LCMS-IT-TOF and UPLC-MS/MS methods,4 kinds of progesterone hormones showed good linearities in the range of 1.0?100.0 2?g/L and high correlation coefficents(r~2>0.99).The detction limits were in the range of 0.2-0.3 ?g/kg and the quantitation limits were in the range of 0.6-0.9?g/kg.The mean recoveries at three spiked level ranged from 81.2%?99.7%by LCMS-IT-TOF method,and ranged from 71.7%?84.7%by UPLC-MS/MS method.(4)A method for the determination of 8 kinds of estrogenic hormones in duck meat by Gel Permeation Chromatography as clean up step and mass spectrometry as detection step.The protein of the residues was precipitated by acetonitrile and ethyl acetate(1:1,v/v),and then residues were extracted again by ethyl acetate.The estrogenic hormones were analyzed in ESI-mode after gel permeation chromatography clean-up.The result indicate that using the LCMS-IT-TOF and UPLC-MS/MS methods,8 kinds of estrogenichormones showed good linearities in the range of 1.0?100.0?g/L and high correlation coefficents(r~2>0.99).The detction limits were in the range of 0.3?0.6 ?g/kg and the quantitation limits were in the range of 0.9?1.8 ?g/kg.The mean recoveries at three spiked level ranged from 77.7%?113.2%by LCMS-IT-TOF method,and ranged from 81.2%?108.7%by UPLC-MS/MS method.(5)The multiple mass spectrums of 16 kinds of estrogenic and progesterone hormones,including 8 kinds of estrogen hormones,4 kinds of progesterone hormones and 4kinds of isotope internal standard,were got using LCMS-IT-TOF,and the ACDLabs MS library were established.The rapid process of screening and identification of estrogenic and progesterone hormones in food were established.In conclusion,the new developed methods using LCMS-IT-TOF and UPLC-MS/MS were sensitive,effective and reliable for the quantitative and qualitative analysis of estrogenic and progesterone hormones in infant formul,eggs and duck meat The methods were suitable for the screening and identification of estrogenic and progesterone hormones in foods.