PMID- 19467664 OWN - NLM STAT- MEDLINE DCOM- 20100106 LR - 20191210 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1216 IP - 46 DP - 2009 Nov 13 TI - Development of a rapid, multi-class method for the confirmatory analysis of anti-inflammatory drugs in bovine milk using liquid chromatography tandem mass spectrometry. PG - 8132-40 LID - 10.1016/j.chroma.2009.04.078 [doi] AB - A rapid liquid chromatography tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the simultaneous identification, confirmation and quantitation of seven licensed anti-inflammatory drugs (AIDs) in bovine milk. The method was validated in accordance with the criteria defined in Commission Decision 2002/657/EC. Two classes of AIDs were investigated, corticosteroids and non-steroidal anti-inflammatory drugs (NSAIDs). The developed method is capable of detecting and confirming dexamethasone (DXM), betamethasone (BTM), prednisolone (PRED), tolfenamic acid (TLF), 5-hydroxy flunixin (5-OH-FLU), meloxicam (MLX) and 4-methyl amino antipyrine (4-MAA) at their associated maximum residue limits (MRLs). These compounds represent all the corticosteroids and NSAIDs licensed for use in bovine animals producing milk for human consumption. These compounds have never been analysed before in the same method and also 4-methyl amino antipyrine has never been analysed with the other licensed NSAIDs. The method can be considered rapid as permits the analysis of up to 30 samples in one day. Milk samples are extracted with acetonitrile; sodium chloride is added to aid partition of the milk and acetonitrile mixture. The acetonitrile extract is then subjected to liquid-liquid purification by the addition of hexane. The purified extract is finally evaporated to dryness and reconstituted in a water/acetonitrile mixture and determination is carried out by LC-MS/MS. Decision limit (CCalpha) values and detection capability (CCbeta) values have been established for each compound. FAU - Malone, E M AU - Malone EM AD - The State Laboratory, Young's Cross, Celbridge, Co Kildare, Ireland. edward.malone@statelab.ie FAU - Dowling, G AU - Dowling G FAU - Elliott, C T AU - Elliott CT FAU - Kennedy, D G AU - Kennedy DG FAU - Regan, L AU - Regan L LA - eng PT - Evaluation Study PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20090504 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Anti-Inflammatory Agents) SB - IM MH - Animals MH - Anti-Inflammatory Agents/*chemistry MH - Cattle MH - Chromatography, Liquid/*methods MH - Milk/*chemistry MH - Tandem Mass Spectrometry/*methods EDAT- 2009/05/27 09:00 MHDA- 2010/01/07 06:00 CRDT- 2009/05/27 09:00 PHST- 2009/01/04 00:00 [received] PHST- 2009/03/31 00:00 [revised] PHST- 2009/04/24 00:00 [accepted] PHST- 2009/05/27 09:00 [entrez] PHST- 2009/05/27 09:00 [pubmed] PHST- 2010/01/07 06:00 [medline] AID - S0021-9673(09)00668-2 [pii] AID - 10.1016/j.chroma.2009.04.078 [doi] PST - ppublish SO - J Chromatogr A. 2009 Nov 13;1216(46):8132-40. doi: 10.1016/j.chroma.2009.04.078. Epub 2009 May 4.