NDLI: Quantitative Determination and Confirmation of Five Synthetic Glucocorticoid Residues in Milk Powder by Gel Permeation Chromatography–Liquid Chromatography

Content Provider	Springer Nature Link
Author	Sun, Hanwen Kang, Zhansheng Li, Hui Zhang, Jingxuan Lv, Yunkai
Copyright Year	2011
Abstract	A new method for multi-residue determination of five synthetic glucocorticoids (betamethasone, dexamethasone, prednisone, prednisolone, and hydrocortisone) in milk powder is developed. The glucocorticoids in the samples were extracted with tert-butyl methyl ether under ultrasonication incubation, and then cleaned up through gel permeation chromatography. After C18 LC gradient elution separation using acetonitrile with 0.1% formic acid as a mobile phase, the eluents were determined by liquid chromatography–tandem mass spectrometry with multiple reaction monitoring and positive ionization modes. The effective separation for the five glucocorticoids was achieved. The limit of quantification of the method for testing five glucocorticoids in milk powder was in the range from 0.2 to 0.5 μg kg$^{−1}$, which was lower than the maximum residue limits established by European Union for glucocorticoids in foods. Experiments on spiked samples of milk powder showed that the mean recoveries at addition level of 1.0, 3.0, and 5.0 μg kg$^{−1}$ were in the range of 71.2% and 103%, and the relative standard deviation ranged from 4.7% to 16.8%. The calibration curves for these drugs between 1.0 and 100 μg l$^{−1}$ showed good linearity, with correlation coefficient (r) more than 0.999. The real sample test showed that this method is sensitive and accurate. It can be used for qualitative and quantitative determination of studied glucocorticoid residues in milk powder samples.
Starting Page	643
Ending Page	650
Page Count	8
File Format	PDF
ISSN	19369751
Journal	Food Analytical Methods
Volume Number	5
Issue Number	4
e-ISSN	1936976X
Language	English
Publisher	Springer-Verlag
Publisher Date	2011-09-08
Publisher Place	New York
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Gel permeation chromatography Liquid chromatography–tandem mass spectrometry Glucocorticoids Milk powder Chemistry/Food Science Microbiology Analytical Chemistry Food Science
Content Type	Text
Resource Type	Article
Subject	Analytical Chemistry Safety Research Safety, Risk, Reliability and Quality Applied Microbiology and Biotechnology Food Science

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