Development and validation of a liquid chromatographic-tandem mass spectrometric method for determination of eleven coccidiostats in milk

被引:41
作者
Nasz, Szilard [1 ]
Debreczeni, Lajos [2 ]
Rikker, Tamas [3 ]
Eke, Zsuzsanna [1 ,3 ]
机构
[1] Eotvos Lorand Univ, Joint Res & Training Lab Separat Tech, H-1117 Budapest, Hungary
[2] Feed Invest Natl Reference Lab, Food & Feed Safety Directorate, Cent Agr Off, H-1144 Budapest, Hungary
[3] Wessling Int Res & Educ Ctr, H-1047 Budapest, Hungary
关键词
LC-MS-MS; Coccidiostats; Milk; Validation; Solid phase extraction; IONOPHORE COCCIDIOSTATS; POULTRY FEEDS; TARGETED FEED; EGGS; NICARBAZIN; MONENSIN;
D O I
10.1016/j.foodchem.2012.01.022
中图分类号
O69 [应用化学];
学科分类号
081704 ;
摘要
A reversed phase liquid chromatographic-tandem mass spectrometric method with simple solvent extraction and purification by solid phase extraction (SPE) has been developed for the determination of coccidiostats in milk. For sample preparation matrix solid phase dispersion, extraction by organic solvent and SPE with different cartridges were also tested. The compounds determined include lasalocid, narasin, salinomycin, monensin, semduramicin, maduramicin, robenidine, decoquinate, halofuginone, nicarbazin and diclazuril. Main steps of the method are addition of acetonitrile to the milk samples, centrifugation, removal of matrix by SPE, concentration by evaporation and LC-MS-MS determination. During a 15 min time segmented chromatographic run compounds are ionised either positively or negatively. Calculated recoveries range between 77.1% and 118.2%. Maximum levels are in the range of 1-20 mu g/kg. The developed method was validated in line with the requirements of Commission Decision 2002/657/EC (2002). It is applicable for control of coccidiostat residues in milk as indicated in Regulation 124/2009/EC (2009). (C) 2012 Elsevier Ltd. All rights reserved.
引用
收藏
页码:536 / 543
页数:8
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