title: Development of a liquid chromatography-tandem mass spectrometry with pressurized liquid extraction for determination of glucocorticoid residues in edible tissues.
abstract: A multi-residues method using pressurized liquid extraction (PLE) and liquid chromatography combined with mass spectrometry (LC-MS/MS) has been developed for determination of eight glucocorticoids (prednisone, prednisolone, hydrocortisone, methylprednisolone, dexamethasone, betamethasone, beclomethasone, fludrocortisone) in muscle of swine, cattle, and sheep. Parameters affecting PLE extraction including extraction solvent, extraction temperature, extraction pressure and extraction cycles were optimized. The optimized method employed 11 ml extraction cells, hexane-ethyl acetate (50:50, v/v) as extraction solvent, 1500 psi of extraction pressure and 50°C of extraction temperature. The samples were detected by LC-ESI-MS/MS in negative mode with selected reaction monitoring (SRM) mode. The recovery of glucocorticoids spiked at levels of 0.5-6 μg kg(-1) ranged from 70.1% to 103.1%; the between-day relative standard deviations were no more than 9.6%. The limits of quantification were 0.5-2 μg kg(-1) in muscle. The results demonstrated that the method is simple, fast, robust, and suitable for identification and quantification of glucocorticoids residues in foods of animal origin.
authors.affiliation: MAO Key Laboratory of Food Safety Evaluation/National Reference Laboratory of Veterinary Drug Residues (HZAU), Huazhong Agricultural University, Wuhan, Hubei 430070, China.
authors.forename: Dongmei
authors.initials: D
authors.lastname: Chen
authors.forename: Yanfei
authors.initials: Y
authors.lastname: Tao
authors.forename: Zhaoying
authors.initials: Z
authors.lastname: Liu
authors.forename: Huahai
authors.initials: H
authors.lastname: Zhang
authors.forename: Zhenli
authors.initials: Z
authors.lastname: Liu
authors.forename: Yulian
authors.initials: Y
authors.lastname: Wang
authors.forename: Lingli
authors.initials: L
authors.lastname: Huang
authors.forename: Yuanhu
authors.initials: Y
authors.lastname: Pan
authors.forename: Dapeng
authors.initials: D
authors.lastname: Peng
authors.forename: Menghong
authors.initials: M
authors.lastname: Dai
authors.forename: Xu
authors.initials: X
authors.lastname: Wang
authors.forename: Zonghui
authors.initials: Z
authors.lastname: Yuan
mesh_terms: D000085:Acetates; D000818:Animals; D002417:Cattle; D005591:Chemical Fractionation / Q000379:methods*; D002853:Chromatography, Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis*; D005504:Food Analysis / Q000379:methods*; D005938:Glucocorticoids / Q000032:analysis* / Q000737:chemistry; D006586:Hexanes; D008460:Meat / Q000032:analysis*; D018482:Muscle, Skeletal / Q000737:chemistry; D011312:Pressure; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013552:Swine; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013696:Temperature
chemical_list: D000085:Acetates; D005938:Glucocorticoids; D006586:Hexanes; C007650:ethyl acetate