Multiresidue analysis of glucocorticoids in milk by LC-MS/MS with low-temperature purification and dispersive solid-phase extraction

文献类型： 外文期刊

第一作者： Ma, Lili

作者： Ma, Lili;Fan, Xiaojing;Jia, Li;Wang, Jiaqi;Wang, Suli;Zhao, Liuwei

作者机构：

关键词： dispersive solid-phase extraction;glucocorticoids;low-temperature purification;milk

期刊名称：JOURNAL OF SEPARATION SCIENCE （ 影响因子：3.645； 五年影响因子：2.943 ）

ISSN：

年卷期：

页码：

收录情况： SCI

摘要： A multiresidue method for the determination of 12 glucocorticoids (clobetasol propionate, budesonide, triamcinolone, triamcinolone acetonide, fludrocortisone acetate, flumethasone, beclomethasone, prednisone acetate, 6-alpha-methylprednisolone, hydrocortisone, cortisone, and prednisone) in bovine milk was developed using liquid chromatography with tandem mass spectrometry. Isoflupredone was used as an internal standard. Milk samples were treated with ethyl acetate to extract glucocorticoids and were frozen at -20 degrees C for 6 h to precipitate fat. The extract was dried under nitrogen, and residues were dissolved in an acetonitrile/water solution. A further clean-up step was used by dispersive solid-phase extraction, with octadecyl silica and primary secondary amine as the absorbents. The recoveries of glucocorticoids spiked at 0.5, 1.0, 10.0 mu g/kg ranged from 75.7 to 117.3%, except for clobetasol propionate and budesonide (16.1-49.5%). The limits of quantification were 0.01-0.5 mu g/kg in milk. This method has been successfully applied in real samples. The results demonstrated that this method is simple, robust, and suitable for identification of glucocorticoid residues in milk.

分类号： O6

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