Beijing Center for Physical and Chemical Analysis, Beijing Engineering Research Center of Food Safety Analysis, Beijing, China.
College of Science, Food Safety Research Center, Hebei North University, Zhangjiakou, China.
J Sep Sci. 2017 Jul;40(13):2759-2768. doi: 10.1002/jssc.201700064. Epub 2017 Jun 14.
A multiresidue method for the determination of 12 glucocorticoids (clobetasol propionate, budesonide, triamcinolone, triamcinolone acetonide, fludrocortisone acetate, flumethasone, beclomethasone, prednisone acetate, 6-α-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°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 μg/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 μg/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.
一种用于牛奶中 12 种糖皮质激素（氯倍他索丙酸酯、布地奈德、曲安西龙、曲安西龙醋酸酯、醋酸氟氢可的松、氟替卡松、倍他米松、醋酸泼尼松龙、6-α-甲基泼尼松龙、氢化可的松、可的松和泼尼松）测定的多残留方法已经开发出来，该方法使用液相色谱-串联质谱法。异氟泼尼酮被用作内标。牛奶样品用乙酸乙酯处理以提取糖皮质激素，并在-20°C下冷冻 6 小时以沉淀脂肪。提取物在氮气下干燥，残留物溶解在乙腈/水溶液中。进一步使用分散固相萃取进行净化，十八烷基硅烷和伯仲胺作为吸附剂。在 0.5、1.0、10.0 μg/kg 浓度下添加的糖皮质激素的回收率在 75.7%至 117.3%之间，除了氯倍他索丙酸酯和布地奈德（16.1%-49.5%）。牛奶中该方法的定量限为 0.01-0.5μg/kg。该方法已成功应用于实际样品。结果表明，该方法简单、稳健，适用于牛奶中糖皮质激素残留的鉴定。
