Hurtaud-Pessel Dominique, Couëdor Pierrick, Verdon Eric, Dowell Dawn
ANSES, French Agency for Food, Environmental and Occupational Health Safety, Fougères Laboratory, Veterinary Drug Residues Unit, EU-RL for Antibiotic and Dye Residues, La Haute Marche, Javen6, BP 90203, 35302 Fougères, France.
J AOAC Int. 2013 Sep-Oct;96(5):1152-7. doi: 10.5740/jaoacint.13-142.
During the AOAC Annual Meeting held from September 30 to October 3, 2012 in Las Vegas, NV, the Expert Review Panel (ERP) on Veterinary Drug Residues reviewed data for the method for determination of residues of three triphenylmethane dyes and their metabolites (malachite green, leuco malachite green, crystal violet, leuco crystal violet, and brilliant green) in aquaculture products by LC/MS/MS, previously published in the Journal of Chromatography A 1218, 1632-1645 (2006). The method data were reviewed and compared to the standard method performance requirements (SMPRs) found in SMPR 2009.001, published in AOAC's Official Methods of Analysis, 19th Ed. (2012). The ERP determined that the data were acceptable, and the method was approved AOAC Official First Action. The method uses acetonitrile to isolate the analyte from the matrix. Then determination is conducted by LCIMS/MS with positive electrospray ionization. Accuracy ranged from 100.1 to 109.8% for samples fortified at levels of 0.5, 0.75, 1.0, and 2.0 microg/kg. Precision ranged from 2.0 to 10.3% RSD for the intraday samples and 1.9 to 10.6% for the interday samples analyzed over 3 days. The described method is designed to accurately operate in the analytical range from 0.5 to 2 microg/kg, where the minimum required performance limit for laboratories has been fixed in the European Union at 2.0 microg/kg for these banned substances and their metabolites. Upper levels of concentrations (1-100 microg/kg) can be analyzed depending on the different optional calibrations used.
2012年9月30日至10月3日在内华达州拉斯维加斯举行的美国官方分析化学师协会（AOAC）年会上，兽药残留专家评审小组（ERP）审查了此前发表于《色谱A杂志》1218卷，1632 - 1645页（2006年）的关于用液相色谱/串联质谱法测定水产养殖产品中三种三苯甲烷染料及其代谢物（孔雀石绿、无色孔雀石绿、结晶紫、无色结晶紫和亮绿）残留量的方法的数据。该方法数据经过审查，并与《AOAC官方分析方法》第19版（2012年）中SMPR 2009.001里的标准方法性能要求（SMPR）进行了比较。ERP认定这些数据是可接受的，该方法被批准为AOAC官方首次行动方法。该方法使用乙腈从基质中分离分析物，然后通过带有正电喷雾电离的液相色谱/串联质谱法进行测定。对于添加水平为0.5、0.75、1.0和2.0微克/千克的样品，回收率范围为100.1%至109.8%。日内样品的精密度相对标准偏差（RSD）范围为2.0%至10.3%，为期3天分析的日间样品的精密度RSD范围为1.9%至10.6%。所描述的方法设计用于在0.5至2微克/千克的分析范围内准确运行，在欧盟，这些被禁止物质及其代谢物的实验室最低要求性能限已设定为2.0微克/千克。根据所使用的不同可选校准方法，可以分析更高浓度水平（1 - 100微克/千克）的样品。
