Rapid simultaneous determination of dexamethasone and betamethasone in milk by liquid chromatography tandem mass spectrometry with isotope dilution

被引：36
作者：
Li Cun [2 ]
Wu Yinliang [1 ]
Yang Ting
Zhang Yan
机构：
[1] Ningbo Acad Agr Sci, Ningbo Agr Prod Qual Detector Ctr, Ningbo 315040, Zhejiang, Peoples R China
[2] Hebei Univ Engn, Coll Agr, Handan 056038, Peoples R China
来源：
JOURNAL OF CHROMATOGRAPHY A | 2010年 / 1217卷 / 03期
关键词：
Dexamethasone; Betamethasone; Milk; HPLC-MS/MS; Isotope dilution; NEGATIVE CHEMICAL-IONIZATION; BOVINE LIVER; QUANTITATIVE-DETERMINATION; SYNTHETIC CORTICOSTEROIDS; GLUCOCORTICOID RESIDUES; GAS-CHROMATOGRAPHY; URINE; OPTIMIZATION; CONFIRMATION; EXTRACTION;
D O I：
10.1016/j.chroma.2009.12.015
中图分类号：
Q5 [生物化学];
学科分类号：
071010 ; 081704 ;
摘要：
A simple, sensitive and reliable analytical method for the rapid simultaneous determination of dexamethasone and betamethasone in milk by high performance liquid chromatography-negative electrospray ionization tandem mass spectrometry (HPLC-NESI-MS/MS) with isotope dilution was developed. Samples were directly purified through C-18 cartridge. Then the eluate was dried under nitrogen and residues were dissolved in mobile phase. Samples were analyzed by HPLC-MS/MS on a Hypercarb graphite column with a mixture of acetonitrile-water-formic acid as mobile phase. The samples were quantified using dexamethasone-D-4 as an internal standard. The procedure was validated according to the European Union regulation 2002/657/EC determining specificity, decision limit (CC alpha), detection capability (CC beta), trueness, precision, linearity and stability. The method is demonstrated to be suitable for the determination of dexamethasone and betamethasone in milk. The total time required for the analysis of one sample was about 35 min. (C) 2009 Elsevier B.V. All rights reserved.
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收藏
页码：411 / 414
页数：4
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