Istituto Zooprofilattico Sperimentale del Mezzogiorno, Via Salute, 2, 80055 Portici (NA), Italy.
Rapid Commun Mass Spectrom. 2010 Apr 15;24(7):1017-24. doi: 10.1002/rcm.4478.
Flavomycin complex is an antibiotic banned in the European Union as an additive in feed stuffs. As a consequence, the monitoring programmes for official control within the Community require analysis of feeds for possible illegal use of flavomycin. A method for unambiguous identification and quantification of moenomycin A, the main pharmacologically active component of flamomycin complex, in several feeds by liquid chromatography coupled to electrospray ion trap mass spectrometry (LC/ESI-MS/MS) is herein described for the first time. The method was developed to be used as a confirmative analytical tool for the network of Italian official control laboratories; both the singly and doubly charged molecular ions were observed as precursor ions, from which four product ions were selected for both quantitative analysis and unambiguous identification of moenomycin A. The method was in-house validated for feeds in the concentration range 0.50-30.0 microg/g, according to the Regulation 882/2004/EC requirements. Mean recoveries ranging between 83.9-94.2% and relative standard deviations <23% account for method trueness and repeatability, respectively. Moreover, other analytical performance parameters, i.e. method specificity, ruggedness, the linearity of detector response, the limit of quantification (LOQ), the limit of detection (LOD), and measurement uncertainty were evaluated and reported. The ion trap LC/ESI-MS/MS method is highly selective and reliable; high drug recovery, good reproducibility and an LOQ down to 0.10 microg/g guarantee its applicability for confirmatory purposes in the official control activity in Italy.
flavomycin 复合物是一种抗生素,因其作为饲料添加剂在欧盟被禁用。因此,欧盟共同体的官方监测计划要求对饲料进行分析,以检测是否存在非法使用 flavomycin 的情况。本文首次描述了一种利用液相色谱-电喷雾串联质谱法(LC/ESI-MS/MS)对多种饲料中主要药效成分莫能菌素 A 进行定性和定量分析的方法。该方法旨在作为意大利官方控制实验室网络的确认性分析工具;可观察到单电荷和双电荷分子离子作为前体离子,从中选择四个产物离子,用于莫能菌素 A 的定量分析和定性确认。该方法按照 2004 年 8 月 28 日理事会第 882/2004/EC 号法规要求,对浓度范围在 0.50-30.0 μg/g 的饲料进行了内部验证。平均回收率在 83.9-94.2%之间,相对标准偏差 <23%,分别代表了方法的准确度和重复性。此外,还评估并报告了其他分析性能参数,如方法特异性、耐用性、检测器响应的线性、定量限(LOQ)、检测限(LOD)和测量不确定度。该离子阱 LC/ESI-MS/MS 方法具有高度选择性和可靠性;高药物回收率、良好的重现性和低至 0.10 μg/g 的 LOQ 保证了其在意大利官方控制活动中的确证目的的适用性。