Dowling G, Gallo P, Fabbrocino S, Serpe L, Regan L
The State Laboratory, Young's Cross, Celbridge, Ireland.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2008 Dec;25(12):1497-508. doi: 10.1080/02652030802383160.
A method has been developed to analyse for ibuprofen (IBP), ketoprofen (KPF), diclofenac (DCF) and phenylbutazone (PBZ) residues in bovine milk. Milk samples were extracted with acetonitrile and sample extracts were purified on Isolute C(18) solid-phase extraction cartridges. Aliquots were analysed by gas chromatography-tandem mass spectrometry (GC-MS/MS). The method was validated in bovine milk, according to the criteria defined in Commission Decision 2002/657/EC. The decision limits (CCalpha were 0.59, 2.69, 0.90 and 0.70 ng ml(-1), respectively, for IBP, KPF, DCF and PBZ, and detection capabilities (CCbeta) of 1.01, 4.58, 1.54 and 1.19 ng ml(-1), respectively, were obtained. The measurement uncertainty of the method was 17.8%, 80.9%, 28.2% and 20.2% for IBP, KPF, DCF and PBZ, respectively. Fortifying bovine milk samples (n = 18) in three separate assays show the accuracy of the method to be between 104% and 112%. The precision of the method, expressed as relative standard deviations for the within-laboratory reproducibility at the three levels of fortification (5, 7.5 and 10 ng ml(-1)) was less than 8% for IBP, DCF and PBZ, respectively. Poor precision was obtained for KPF with a relative standard deviation of 28%.
已开发出一种分析牛乳中布洛芬（IBP）、酮洛芬（KPF）、双氯芬酸（DCF）和保泰松（PBZ）残留量的方法。牛奶样品用乙腈萃取，样品萃取液在Isolute C(18)固相萃取柱上进行净化。取等分试样通过气相色谱 - 串联质谱法（GC-MS/MS）进行分析。根据欧盟委员会第2002/657/EC号决定中规定的标准，该方法在牛乳中得到验证。对于IBP、KPF、DCF和PBZ，测定下限（CCα）分别为0.59、2.69、0.90和0.70 ng ml(-1)，检测能力（CCβ）分别为1.01、4.58、1.54和1.19 ng ml(-1)。该方法的测量不确定度对于IBP、KPF、DCF和PBZ分别为17.8%、80.9%、28.2%和20.2%。在三次单独的分析中对牛乳样品（n = 18）进行加标显示该方法的准确度在104%至112%之间。该方法的精密度，以在三个加标水平（5、7.5和10 ng ml(-1)）下实验室内部再现性的相对标准偏差表示，对于IBP、DCF和PBZ分别小于8%。对于KPF，精密度较差，相对标准偏差为28%。
