Laboratori de Bromatologia i Toxicologia, Facultat de Farmacia, Universitat de Valéncia, Burjassot, Spain.
J Sep Sci. 2010 Mar;33(4-5):522-9. doi: 10.1002/jssc.200900682.
A simple method for the simultaneous determination of dihydrostreptomycin, spectinomycin, spiramycin, streptomycin, tilmicosin, and tylosin in meat has been developed using pressurized liquid extraction and LC-triple quadrupole MS (LC-ESI-MS/MS). The pressurized liquid extraction operational parameters were optimized and no protein precipitating and fat removing steps were required. A gradient HPLC separation was developed with ion-pair mobile phases consisting of aqueous 1 mM heptafluorobutyric acid water and methanol. Protonated molecules were used as precursor ions for CID. Data acquisition under MS/MS was achieved by applying multiple reaction monitoring of three fragment ion transitions to provide a high degree of sensitivity and specificity. Dirithromycin and sisomycin were selected as internal standards. A validation study was conducted for these antibiotics in poultry meat samples. All selected compounds could be detected (monitoring ions by multiple reaction monitoring) in meat samples at amounts below the regulatory level of concern. Using the internal standards, pressurized liquid extraction recovery rates were from 70 to 96% (RSD 12-25%). LC-ESI-MS/MS method detection limits of the selected antibiotics were 1-6 microg/kg. Good method reproducibility was found by intra- and inter-day precisions at maximum residue level, yielding the RSDs less than 15 and 16%, respectively.
一种使用加压液体萃取和 LC-三重四极杆 MS（LC-ESI-MS/MS）同时测定肉中二氢链霉素、壮观霉素、螺旋霉素、链霉素、替米考星和泰乐菌素的简单方法已经开发出来。优化了加压液体萃取操作参数，无需进行蛋白质沉淀和脂肪去除步骤。开发了一种梯度 HPLC 分离方法，离子对流动相由含 1mM 七氟丁酸的水和甲醇组成。质子化分子被用作 CID 的前体离子。通过应用三个片段离子跃迁的多重反应监测实现了 MS/MS 下的数据采集，从而提供了高度的灵敏度和特异性。地红霉素和西索米星被选为内标。对这些抗生素在禽肉样品中的验证研究进行了。所有选定的化合物都可以在肉样中检测到（通过多重反应监测监测离子），其含量低于关注的监管限量。使用内标，加压液体萃取回收率在 70%至 96%之间（RSD 为 12%至 25%）。选定抗生素的 LC-ESI-MS/MS 方法检测限为 1-6μg/kg。在最大残留水平下，通过日内和日间精密度发现了良好的方法重现性，其 RSD 分别小于 15%和 16%。
