Di Rocco M, Moloney M, O'Beirne T, Earley S, Berendsen B, Furey A, Danaher M
Food Safety Department, Teagasc Food Research Centre, Ashtown, Dublin 15, Ireland; Mass Spectrometry Research Group, Department of Physical Sciences, Cork Institute of Technology, Bishopstown, Cork, Ireland.
Food Safety Department, Teagasc Food Research Centre, Ashtown, Dublin 15, Ireland.
J Chromatogr A. 2017 Jun 2;1500:121-135. doi: 10.1016/j.chroma.2017.04.022. Epub 2017 Apr 12.
A method was developed for the confirmatory and quantitative analysis of 30 β-lactam antibiotic residues in bovine muscle. The method includes 12 penicillins (amoxicillin, ampicillin, cloxacillin, dicloxacillin, mecillinam, methicillin, nafcillin, oxacillin, penicillin G, penicillin V, piperacillin, ticarcillin), 12 cephalosporins (cefacetrile, cefadroxil, cephalexin, cefalonium, cefazolin, cefoperazone, cefotaxime, cefquinome, cefuroxime, desacetyl cephapirin, desfuroylceftiofur cysteine disulfide, desfuroylceftiofur dimer), five carbapenems (biapenem, doripenem, ertapenem, imipenem, meropenem) and faropenem. Samples were extracted using a simple solvent extraction with acetonitrile:water (80:20, v/v) and C dispersive solid-phase extraction (d-SPE) clean-up, followed by ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) detection. Chromatography was performed on a reversed phase CSH C column, using a binary gradient separation comprising of 0.01% formic acid and 0.2mM ammonium acetate in water (mobile phase A) and 0.01% formic acid in acetonitrile (mobile phase B). The mass spectrometer was operated in the positive electrospray ionisation mode (ESI(+)). Validation was performed following the 2002/657/EC guidelines. Trueness ranged between 69% and 143% and precision ranged between 2.0% and 29.9% under within-laboratory reproducibility conditions. The developed method uses minimal sample preparation and 30 test samples can be analysed by a single analyst in a single day. To the best of our knowledge, this is the first method for carbapenems in foodstuff that does not require derivatisation.
开发了一种用于牛肌肉中30种β-内酰胺类抗生素残留的确证和定量分析方法。该方法包括12种青霉素（阿莫西林、氨苄西林、氯唑西林、双氯西林、美西林、甲氧西林、萘夫西林、苯唑西林、青霉素G、青霉素V、哌拉西林、替卡西林）、12种头孢菌素（头孢乙腈、头孢羟氨苄、头孢氨苄、头孢洛宁、头孢唑林、头孢哌酮、头孢噻肟、头孢喹肟、头孢呋辛、去乙酰头孢匹林、去呋喃甲酰头孢噻呋半胱氨酸二硫化物、去呋喃甲酰头孢噻呋二聚体）、5种碳青霉烯类抗生素（比阿培南、多立培南、厄他培南、亚胺培南、美罗培南）和法罗培南。样品采用乙腈:水（80:20，v/v）的简单溶剂萃取和C分散固相萃取（d-SPE）净化，随后进行超高效液相色谱-串联质谱（UHPLC-MS/MS）检测。色谱分析在反相CSH C柱上进行，使用二元梯度分离，流动相A为含0.01%甲酸和0.2 mM醋酸铵的水溶液，流动相B为含0.01%甲酸的乙腈溶液。质谱仪在正电喷雾电离模式（ESI(+)）下运行。按照2002/657/EC指南进行验证。在实验室内部重现性条件下，准确度在69%至143%之间，精密度在2.0%至29.9%之间。所开发的方法样品前处理简单，一名分析人员一天内可分析30个测试样品。据我们所知，这是第一种用于食品中碳青霉烯类抗生素且无需衍生化的方法。
