National Reference Laboratory of Veterinary Drug Residues (HZAU)/MOA, Huazhong Agricultural University, Wuhan, Hubei 430070, China.
Food Chem. 2012 Nov 15;135(2):676-83. doi: 10.1016/j.foodchem.2012.04.086. Epub 2012 Apr 24.
An automated method has been developed for the simultaneous quantification of 15 aminoglycosides in muscle, liver (pigs, chicken and cattle), kidney (pigs and cattle), cow milk, and hen eggs by liquid chromatography tandem mass spectrometry. Homogenized samples were extracted by monopotassium phosphate buffer (including ethylene diamine tetraacetic acid), and cleaned up with auto solid-phase extraction by carboxylic acid cartridges. The analytes were separated by a specialized column for aminoglycosides, and eluted with trifluoroacetic acid and acetonitrile. The decision limits (CCα) of apramycin, gentamycin, tobramycin, paromomycin, hygromycin, neomycin, kanamycin, sisomicin, netilmicin, ribostamycin, kasugamycin, amikacin, streptomycin, dihydrostreptomycin and spectinomycin were ranged from 8.1 to 11.8 μg/kg and detection capabilities (CCβ) from 16.4 to 21.8 μg/kg. High correlation coefficients (r(2)>0.99) of calibration curves for the analytes were obtained within linear from 20 to 1000 μg/kg. Reasonable recoveries (71-108%) were demonstrated with excellent relative standard deviation (RSD). This method is simple pretreatment, rapid determination and high sensitivity, which can be used in the determination of multi-aminoglycosides in complex samples.
已开发出一种自动化方法，用于通过液相色谱串联质谱法同时定量检测肌肉、肝脏（猪、鸡和牛）、肾脏（猪和牛）、牛奶和鸡蛋中的 15 种氨基糖苷类药物。将匀浆样品用单磷酸钾缓冲液（含乙二胺四乙酸）提取，并用羧酸基固相萃取小柱进行净化。分析物用氨基糖苷类专用柱分离，用三氟乙酸和乙腈洗脱。大观霉素、庆大霉素、妥布霉素、巴龙霉素、潮霉素、新霉素、卡那霉素、西索米星、奈替米星、核糖霉素、井冈霉素、阿米卡星、链霉素、双氢链霉素和壮观霉素的决定限（CCα）范围为 8.1 至 11.8μg/kg，检测能力（CCβ）范围为 16.4 至 21.8μg/kg。在 20 至 1000μg/kg 的线性范围内，分析物的校准曲线具有较高的相关系数（r²>0.99）。回收率合理（71-108%），相对标准偏差（RSD）良好。该方法预处理简单、测定快速、灵敏度高，可用于复杂样品中多种氨基糖苷类药物的测定。
