水产品中氨基糖苷类药物残留的高效液相色谱-串联质谱检测方法研究

建立了高效液相色谱一串联质谱方法测定水产品中链霉素、双氢链霉素、新霉素、庆大霉素和卡那霉素5种氨基糖苷类抗生素的检测方法。样品中的氨基糖苷类抗生素用磷酸缓冲溶液提取液提取后，经固相萃取进行净化，改进了前处理方法，并对液相和质谱的条件进行了优化。通过实际样品的添加回收试验，方法的定量下限（S／N=10）为10．0μg,／kg。三个添加水平分别为10．0、20．0和50．0μg／kg时，龙虾、鲴鱼的加标回收率均在60％一110％，日内相对标准偏差不超过15．0％。结果表明，该方法简单、灵敏、特异性强，适用于水产品中氨基糖苷类药物残留的检测和确证。

Determination of Aminoglycoside Residue in Aquatic Products using High Performance Liquid Chromatography Tandem Mass Spectrometry

A high performance liquid chromatography- tandem mass spectrometric （HPLC -MS/MS） method was developed for the determination of five aminoglycosides drugs such as streptomycin, dihydrostreptomycin, kanamycin, gentamicin and neomycinb in aquatic products. The aminoglycosides drugs interested were extracted from the samples with phosphate buffer solution and separated by a cation exchange chromatographic column. An improved pre- treatment method was used in this study and the eluent solution types and chromatographic parameters were optimized. In the detection of spiked samples, the detection limite of this method was 10.0 μg/kg （S/N = 10） for the five durgs spiked in fish and crayfish respectively, which can match the requirement of the supervision. The recoveries of the five durgs from fish and crayfish samples spiked with three concentration levels of 10.0, 20.0 and 50.0 μg./kg ranged from 60% to 110% with RSD less than 15.0%. The established method was accurate, sensitive and simple, and was suitable for the quantification of aminoglycosides antibiotics residue in aquatic products.