RESUMO
A method for sensitive analysis of 19 anabolic steroids (AS) in animal oil using enhanced matrix removal lipid (EMR-Lipid) cleanup and ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was developed. Oil samples were extracted with 20 mL of acetonitrile aqueous solution and purified using EMR-Lipid cartridges. The eluent was evaporated to dryness under nitrogen and analyzed by UHPLC-MS/MS using 0.1% formic acid-acetonitrile and 0.1% formic acid-water solutions as the mobile phase via gradient elution. The method effectively removed unwanted matrix co-extractives better than other extraction cleanup techniques while still delivering acceptable recovery results for most of the AS. The established quantification method showed AS recovery in the range of 72.9-110.7% with good precision (relative standard deviation < 15%).
Assuntos
Produtos Biológicos , Espectrometria de Massas em Tandem , Animais , Cromatografia Líquida de Alta Pressão , Lipídeos , Congêneres da TestosteronaRESUMO
A method for rapid screening and quantification of progesterone and progestins in milks by ultrahigh-performance liquid chromatography coupled with quadrupole-high field Orbitrap high-resolution mass spectrometry (UHPLC QE HF HRMS) was established. Milks samples were extracted by acetonitrile + hexane (80 + 20), purified by prime HLB SPE and analyzed by UHPLC QE HF HRMS. The detection limit of progesterone and 21 progestins in milk is between 0.05 µg/kg -0.3 µg /kg, the correlation coefficient of progesterone and progestins in the corresponding concentration range is more than 0.99, recoveries for milk samples are between 80.7% and 108.3% with the relative deviation is less than 15%.The method fulfils the requirements of veterinary drug residue detection validation of EU and China, and successfully applied to detecting the µg/kg level of progesterone and monitoring residual of progestins in real milk.