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Development of a liquid chromatography-tandem mass spectrometry with pressurized liquid extraction for determination of glucocorticoid residues in edible tissues
Authors:Chen Dongmei  Tao Yanfei  Liu Zhaoying  Zhang Huahai  Liu Zhenli  Wang Yulian  Huang Lingli  Pan Yuanhu  Peng Dapeng  Dai Menghong  Wang Xu  Yuan Zonghui
Institution:MAO Key Laboratory of Food Safety Evaluation/National Reference Laboratory of Veterinary Drug Residues (HZAU), Huazhong Agricultural University, Wuhan, Hubei 430070, China.
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.
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