Citation: GONG Lan, CHEN Ming, WEI Xian, ZOU Chun, WANG Ran. Determination of Glucocorticoids in Muscle Tissues by Liquid Chromatography-Electrospray Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(1): 74-80. doi: 10.11895/j.issn.0253-3820.150561 shu

Determination of Glucocorticoids in Muscle Tissues by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

1.
Institute of Food Quality and Safety, Jiangsu Academy of Agricultural Sciences, Key Laboratory of Control Technology and Standard for Agro-product Safety and Quality Ministry of Agriculture, Jiangsu Key Laboratory of Food Quality and Safety-State Key Laboratory Cultivation Base of MOST, Nanjing 210014, China

Corresponding author: WANG Ran,
Received Date: 15 July 2015
Available Online: 14 October 2015
Fund Project: 本文系国家自然科学基金资助项目(No.31302009) (No.31302009)

A method was developed to determine cortisone, cortisol, prednisone and dexamethasone in muscle tissues by high performance liquid chromatography-tandem mass spectrometry (LC-ESI-MS/MS). Deconjugation of glucocorticoids was carried out by enzymatic hydrolysis. These preliminary steps were followed by ethyl acetate extraction and HLB solid phase extraction clean up step for all matrices. Chromatographic separation was achieved on C₈ column and MS/MS data were obtained in the multiple reaction monitoring mode using negative electrospray ionization. Calibration graphs were prepared in the 0.5-50.0 μg/L range and good linearity was achieved (R² ≥ 0.99).The limits of detection (LOQ) and the limits of quantification (LOD) were 0.13-0.25 μg/kg and 0.25-0.50 μg/kg, respectively. Spiking at the levels of 0.5, 5.0 and 10.0 μg/L, the average recovery for glucocorticoids ranged from 74.0% to 101.8%. The relative standard deviations (RSD) were between 0.7%-8.6%.
- Glucocorticoids,
- High performance liquid chromatography tandem mass spectrometry,
- Solid-phase extraction,
- Muscle tissues
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沈阳化工大学材料科学与工程学院沈阳 110142