色谱法
同位素稀释
化学
生牛奶
质谱法
检出限
萃取(化学)
液相色谱-质谱法
串联质谱法
校准曲线
选择性反应监测
高效液相色谱法
残留物(化学)
食品科学
生物化学
作者
P. Li,Y.D. Zhang,S.L. Li,Wen Fang,H.Y. Li,Shanjiang Zhao,Nan Zheng,J.Q. Wang
标识
DOI:10.3168/jds.2018-16187
摘要
We developed a sensitive and selective isotope dilution ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the determination of sulbactam residue in raw bovine milk. Sulbactam and internal standard, sulbactam-d5, were extracted from raw bovine milk via liquid-liquid extraction and enriched with strong anion exchange solid-phase extraction cartridges and finally analyzed by using UPLC-MS/MS with multiple reaction monitoring mode. The method was validated according to European regulations. The calibration curve showed good linearity, with a correlation coefficient of 0.9998. Decision limit and detection capability of sulbactam were determined by matrix calibration curve and were 0.0445 and 0.0517 μg/L, respectively. The recoveries of sulbactam in fortified raw bovine milk ranged from 72.1 to 91.5%, with the intra- and interday relative standard deviations ranging from 3.0 to 18.9%. Furthermore, the developed method was applied to analyzing real raw bovine milk samples collected from dairy farms in Beijing, China. Sulbactam was not determined in all samples. The proposed method could ultimately serve as a methodological foundation for the determination of sulbactam in different types of raw milk and dairy products.
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