| Sex hormones are produced by the animal’s gonads, which have a great effect of promoting mature sexual organs, developing secondary sex characteristics and maintaining sexual functions. The structure of sex hormone is a kind of steroid compound. Secretion of sex hormones is a extremely trace amount, but its regulation effect is obvious and wide-ranging, however, any single ingredient in them can not start a new metabolic process in the body. They are not directly involved in the substantial and energetic transformation but directly or indirectly promote or slow down the original metabolic process in the body, adjusting the speed and direction of the metabolism and physiological process in order to make the body more adapted to the internal and external environmental changes. Metabolism inactivation ways of sex hormones are roughly the same, Sex hormones can shape glucuronide or sulfate compound in the liver, kidney and other organs, and then excrete with the urine or feces. Sex hormones are generally divided into three major categories: androgen, estrogen and progestin.Since 1980s, sex hormones are used to be a additive into the animals’feed to promote the growth of animals, these additives can promote the growth of animal improve the feed conversion, control reproductive cycle and reproductive performance, improve the feed palatability and the animal food flavor. Although the hormones have some effect for animal husbandry, it can also lead the metabolites residue in livestock and poultry products, causing harm to human health. If people eat meat food containing hormones for a long time, even if the content is a trace amount, but the effect is extremely strong, which also can obviously disturb the hormone balance, resulting in women’s menopause disorder, fertility decline, decreasing neonatal immunity, girls with sexual precocity, developmental abnormalities or causing lesions of the male reproductive system, leading to the increase in female breast cancer and ovarian endometriosis incidence, it has strong carcinogenic and teratogenic effects, inducing female diseases such as breast cancer and ovarian cancer, and adverse to human health. Thus, this paper have researched for the adding and residual sex hormones in the feed and biological samples, and established corresponding detection methods with ultra-performance liquid chromatography-quadrupole-time-of-flight mass.The method was established for 9 androgen in feed by ultra-performance liquid chromatography-quadrupole-time-of-flight mass, which extracted by ethyl acetate, then purified the extracting solution by QuEChERS which added the PSA, C18 and MgSO4 to the extracting solution, oscillated and centrifuged, finally the extracting solution was evaporated to dryness under a stream of nitrogen .The residue was dissolved and analyzed on UPLC-QTOF. The method was positive mode, the mobile phase was methanol and 0.1% formic acid-water solution, and the method was optimized for the mobile phase, extraction solution and QuEChERS method. Finally, in the best condition, the limit of quantification of 9 androgen was 10-43μg/kg, and the recovery was 70.0% ~ 99.7% range. This method was much higher than other method in accuracy, and it could better content the qualitative requirement of the residues of drugs in food for the European Union and other developed countries and organizations, and it could effectively avoid false positive results, which had the very good practicability in the food safety control.The method was established for 8 estrogen metabolites in urine by ultra-performance liquid chromatography-quadrupole-time-of-flight mass. The old methods were required enzymatic or derivative for estrogen drugs, and pretreatment was cumbersome, but the direct detection of metabolites of estrogen drugs could avoid these operations, and the mass response of metabolites was higher than the response of estrogen drugs. This method directly purified the urine with C18 SPE, and was negative mode. The mobile phase was acetonitrile and 0.1% formic acid-water solution, and the method was optimized for the choice and eluent of solid phase extraction column. The limit of quantification of 8 estrogen metabolites was 5-10μg/kg, the recovery range was 80.9%~106.7%.This method had simple pretreatment, high accuracy, and it can be effectively applied in the food safety field.The method was established for 8 estrogen metabolites in muscle by ultra-performance liquid chromatography-quadrupole-time-of-flight mass, which was extracted twice with methanol: water (1:1) and methanol: water (4:1), and eliminated the fat with hexane from the extraction, finally purified the extraction with HLB SPE. The method was negative mode, the mobile phase was acetonitrile and 0.1% formic acid-water solution, and the method was optimized for the mobile phase, extraction, SPE column and eluent. The limit of quantification of 8 estrogen metabolites was 5-15μg/kg, the recovery range was 76%~ 98.9%.This method had simple pretreatment, high accuracy, and it can be effectively applied in the food safety field.The method was established for 6 progestin in feeds by ultra-performance liquid chromatography-quadrupole-time-of-flight mass, which was extracted with acetonitrile, and purified with MCX column SPE. The method was positive mode, the mobile phase was acetonitrile and 0.1% formic acid-water solution, and the method was optimized for the mobile phase, SPE column and eluent. The limit of quantification of 6 progestin was 6-10μg/kg, and the recovery range was 83.1%~ 104.5%. This method had simple pretreatment, high accuracy, and it could be effectively applied in the food safety field. |
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