Moretti Simone, Fioroni Laura, Giusepponi Danilo, Pettinacci Laura, Saluti Giorgio, Galarini Roberta
J AOAC Int. 2013 Nov-Dec;96(6):1245-57. doi: 10.5740/jaoacint.12-440.
A confirmatory method for the determination of 11 regulated coccidiostats including the ionophore antibiotics lasalocid, maduramicin, monensin, narasin, salinomycin, and semduramicin and the chemical coccidiostats decoquinate, diclazuril, halofuginone, nicarbazin, and robenidine in animal feed was developed and validated. The procedure was intended for the identification and quantification of the coccidiostats at concentrations relating both to the unintentional carryover as stated in Regulation 574/2011 and to the authorized levels in target feed. The analytes were determined by LC/MS/MS in the positive or negative electrospray ionization mode. The method performance characteristics were estimated in the relevant application field from 0.003 to 200 mg/kg. Validation criteria of linearity, specificity, trueness, precision, LOD, and LOQ along with measurement uncertainty were estimated for all analytes. Absolute and relative matrix effects were also studied. The results proved that the method performance was satisfactory, and it was successfully applied to carryover control by analyzing 165 feed samples collected within regulatory monitoring plans. Finally, since the carryover phenomenon in feed may result in the presence of residues in food products of animal origin, a survey has been carried out on the occurrence of coccidiostats in 167 eggs and animal muscles.
开发并验证了一种用于测定动物饲料中11种受监管抗球虫药的确证方法，这些抗球虫药包括离子载体抗生素拉沙洛西、马杜霉素、莫能菌素、那拉菌素、盐霉素和赛杜霉素，以及化学抗球虫药地考喹酯、地克珠利、常山酮、尼卡巴嗪和氯苯胍。该程序旨在鉴定和定量抗球虫药的浓度，这些浓度既涉及2011年第574号法规所述的无意残留，也涉及目标饲料中的授权水平。通过液相色谱/串联质谱法在正电喷雾电离模式或负电喷雾电离模式下测定分析物。在相关应用领域中，在0.003至200 mg/kg的范围内评估了该方法的性能特征。对所有分析物评估了线性、特异性、准确性、精密度、检测限和定量限以及测量不确定度的验证标准。还研究了绝对和相对基质效应。结果证明该方法的性能令人满意，并且通过分析在监管监测计划中收集的165个饲料样品，该方法成功应用于残留控制。最后，由于饲料中的残留现象可能导致动物源性食品中出现残留物，因此对167个鸡蛋和动物肌肉中的抗球虫药的存在情况进行了调查。
