化学
色谱法
串联质谱法
检出限
选择性反应监测
质谱法
分析物
液相色谱-质谱法
电喷雾电离
残留物(化学)
兽药
固相萃取
生物化学
作者
Caixia Guo,Cuiling Wu,Zihao Zhang,Sijia Tan,Sumeng Chen,Gang Chen
标识
DOI:10.1016/j.chroma.2024.464734
摘要
Abuse of glucocorticoid veterinary drugs in dairy industry can potentially threat milk safety and consequently influence human health. Here a reliable method for determination of 58 glucocorticoid drug residues in milk was established by combining solid phase extraction with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The analytes were extracted with acetonitrile and cleanup with EMR-Lipid lipid removal column. The analytes were chromatographically separated using Poroshell EC-C18 column and acquired by electrospray ionization with multiple-reaction monitoring (MRM) mode. The limit of quantification (S/N ≥ 10) ranged from 0.2 to 2.0 µg/kg and the limit of detection (S/N ≥ 3) ranged from 0.1 to 1.0 µg/kg. Average recoveries were from 71% to 113%, the relative standard deviations (RSDs) were less than 15%, and the correlation coefficients (R2) of calibration curves exceeded 0.99. The method was applied to detect twenty milk products obtained from local supermarkets including ten pasteurized milk and ten UHT milk. Two endogenous glucocorticoids, i.e. hydrocortisone and cortisone were detected but not exceed the maximum residue limits (MRLs).
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