A Simple and Rapid LC-MS/MS Method for Determination of Dexamethasone in Bovine Milk

IF 0.4 Q4 VETERINARY SCIENCES Macedonian Veterinary Review Pub Date : 2020-03-01 DOI:10.2478/macvetrev-2020-0014
M. Ural, A. Kotan
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引用次数: 3

Abstract

Abstract This study provides insight into the development and validation of the simple, rapid and sensitive method of Liquid Chromatography-Tandem Mass Spectrometry for determining the residues of dexamethasone in bovine milk. The maximum residue limit for dexamethasone in bovine milk is 0.3 ng/ml−1. Chromatographic separation was achieved on an Agilent Proshell 120 SB:C18 (2.7µm 100x3.0 mm) column. The bovine milk was extracted with ethyl acetate, and the evaporated elution was dissolved with hexane, water and methanol, and analyzed by the LC-MS/MS method. The mobile phase A was a solution of 5 Mm ammonium formate in water, while the mobile phase B was 0.1% formic acid in acetonitrile. The calibration graphics were prepared within the range of 0.15–0.6 ng/ml−1, and a successful linearity was achieved (r ≥0.999). The limit of detection was 0.016 ng/ml−1. The decision limit (CCα) and detection capability (CCβ) were 0.34 and 0.38 ng/ml−1, respectively.
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高效液相色谱-质谱联用法测定牛奶中地塞米松的含量
摘要本研究深入探讨了液相色谱-串联质谱法测定牛乳中地塞米松残留量的简便、快速、灵敏方法的开发和验证。地塞米松在牛乳中的最大残留限量为0.3 ng/ml−1。在安捷伦Proshell 120 SB:C18(2.7µm 100x3.0 mm)柱上实现色谱分离。用乙酸乙酯提取牛乳,用己烷、水和甲醇溶解蒸发洗脱液,并通过LC-MS/MS方法进行分析。流动相A是5Mm甲酸铵在水中的溶液,而流动相B是0.1%甲酸在乙腈中的溶液。在0.15–0.6 ng/ml−1的范围内制备了校准图,并实现了成功的线性(r≥0.999)。检测限为0.016 ng/ml−1。判定限(CCα)和检测能力(CCβ)分别为0.34和0.38 ng/ml−1。
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来源期刊
Macedonian Veterinary Review
Macedonian Veterinary Review Veterinary-Veterinary (all)
CiteScore
1.00
自引率
0.00%
发文量
20
审稿时长
12 weeks
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