CER Groupe, Division Hormonologie, rue du point du jour, 8-6900 Marloie, Belgium.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2010 Jun;27(6):801-9. doi: 10.1080/19440040903552408.
A multi-residue HPLC-ESI-MS/MS method has been developed for the simultaneous extraction, detection and confirmation of the 11 coccidiostats referenced by Regulation 2009/8/EC (lasalocid sodium, narasin, salinomycin sodium, monensin sodium, semduramicin sodium, maduramicin ammonium alpha, robenidine hydrochloride, decoquinate, halofuginone hydrobromide, nicarbazin, and diclazuril) in feedstuffs at carry-over level. The sensitivity of the method allows quantification and confirmation for all coccidiostats below target concentration. The method was in-house validated and meets all criteria of European legislation (2002/657/EC). The precision of the method was determined under repeatability and within-laboratory reproducibility conditions; RSD(r) and RSD(R) were below the maximum permitted values for every tested concentration. The specificity was checked by analysing representative blank samples and blank samples fortified with potentially interfering substances (benzimidazoles, corticosteroides, triphenylmethane dyes, quinolones, nitrofurans, nitroimidazoles, phenicols); no interference were found. Concerning quantification, a quadratic regression model was fitted to every calibration curve with a regression coefficient r2 above 0.99 on each data set. Finally, the expanded uncertainty U was calculated with data obtained within the laboratory while applying the method during validation and in routine tests.
建立了一种多残留 HPLC-ESI-MS/MS 方法，用于同时提取、检测和确证法规 2009/8/EC（拉沙洛西钠、那拉菌素、盐霉素钠、莫能菌素钠、山度霉素钠、马杜霉素铵α、罗贝林盐酸盐、癸氧喹酯、氢溴酸卤呋酮、尼卡巴嗪和地克珠利）在饲料中的残留水平。该方法的灵敏度允许对所有抗球虫药在目标浓度以下进行定量和确证。该方法经过内部验证，符合欧洲法规（2002/657/EC）的所有标准。方法的精密度在重复性和实验室内部再现性条件下确定；对于每个测试浓度，RSD(r)和 RSD(R)均低于允许的最大值。特异性通过分析代表性空白样品和用潜在干扰物质（苯并咪唑类、皮质甾类、三苯甲烷染料、喹诺酮类、硝基呋喃类、硝基咪唑类、酚类）加标空白样品进行检查；未发现干扰。关于定量，在每个数据集中，每个校准曲线的二次回归模型的回归系数 r2 均大于 0.99。最后，在验证过程中和常规测试中应用该方法时，在实验室内部获得的数据计算出扩展不确定度 U。
