色谱法
化学
重复性
液相色谱-质谱法
质谱法
样品制备
检出限
残留物(化学)
固相萃取
萃取(化学)
串联质谱法
生物化学
作者
Katerina Bousova,Hamide Z. Şenyuva,Klaus Mittendorf
标识
DOI:10.1016/j.chroma.2012.11.067
摘要
A multi-class method for identification and quantification of 36 antibiotics from seven different chemical classes (aminoglycosides, macrolides, lincosamides, sulfonamides, tetracyclines, quinolones and trimethoprim) has been developed by using liquid chromatography–mass spectrometry. The method was optimised for detection of antibiotics in chicken meat. Sample preparation including extraction with a mixture of acetonitrile:2% trichloroacetic acid (45:55, v/v), centrifugation and filtration was followed by on-line clean-up using turbulent flow chromatography. Using this automated on-line technique enabled a larger number of samples to be analysed per day than with a traditional clean-up technique (e.g. solid phase extraction). The optimised method was validated according to the European Commission Directive 2002/657/EC. In-house validation was performed by fortifying the blank matrix at three levels 0.5, 1.0 and 1.5 MRL (maximum residue limit), or respectively, at concentrations as low as possible for substances without an MRL. Precision in terms of repeatability standard deviation ranged from 3 to 28% and recovery values were between 80 and 120% in most cases. All calculated validation parameters including CCα and CCβ were in the compliance with the legislative requirements.
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