Studies On Analytical Methods Of Steroid Hormones Residues In Animal-derived Food

The analysis and detection of hormones residues in animal-derived food is very important for assure food safety and safeguard the consumers' health. This paper aims at using GPC to achieve the effective separation of target compounds from fat molecule, and increase extraction ,then establishing new methods for the determination of hormones residues in animal-derived food by gas chromatography–mass spectrometry or liquid chromatography–tandem mass spectrometry. It includes four chapters as follows:Chapter1: The common knowledge of steroid hormones was summarized briefly. Besides, the sample pretreatment technique and the research status of compartment analysis methods in recent years were reviewed.Chapter2: A gel permeation chromatography solid phase extraction–rapid resolution liquid chromatography–tandem mass spectrometry (GPC–SPE–RRLC–MS/MS ) method was developed for the determination of 9 steroid hormones in beef tissue. The beef samples were enzymatically digested, then extracted and cleaned-up. After C18 RRLC gradient elution separation, the eluents were qualitatively and quantitatively determined under multi-reaction monitoring (MRM) scan type with tandem mass analyzer. The experimental results showed this method is sensitive, and accurate. The proposed method was used for the determination of 9 steroid hormones residues in high-fat and complex sample.Chapter3: A new method was developed for the determination of glucocortiooid residues in milk powder by gel permeation chromatography–liquid chromatography–tandem mass spectrometry (GPC–RRLC–MS/MS).Baseline separation for the five glucocortiooids was achieved. The limit of quantification (LOQ) of the RRLC/MS/MS method used for testing five glucocortiooids in milk powder was in the range from 0.2 to 0.5μg/kg, which were lower than MRL established by European Union for glucocortiooids in foods. The real sample test showed that this method is sensitive and accurate. It can be used for qualitatively and quantitatively determination of studied glucocortiooid residues in milk powder samples.Chapter4: A new method had been developed for effective separation and simultaneous determination of six estrogen residues in infant formula by gas chromatography–mass spectrometry (GC–MS). The infant formula samples were enzymatically digested, then extracted and derivated. After HP-5MS chromatographic column separation, the eluents were detected qualitatively and quantitatively under SIM scan type with mass analyzer.The baseline separation of two isomers (17α-estradiol hemihydrate and 17β-estradiol hemihydrate) of estradiol was achieved by optimizing the heating process. The calibration curves showed good linearity with correlation coefficient (r) of >0.999. This method had been successfully used for the qualitatively and quantitatively determination of the six estrogen residues in infant formula.