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目的建立一种亲水作用色谱串联质谱技术同时检测鱼肉中链霉素和双氢链霉素残留的分析方法。方法以鱼肉为原料,样品经磷酸盐缓冲溶液提取,固相萃取柱净化后,采用亲水作用色谱柱分离,在正离子模式下以电喷雾电离串联质谱进行测定,外标法定量。结果链霉素和双氢链霉素在2.0~50μg/L质量浓度范围内线性关系良好,在10、20、50μg/kg三个加标水平下,方法的回收率为80.2%~97.1%,相对标准偏差为3.3%~7.2%。结论该方法简便、快速、实用、准确,各项技术指标满足国内外法规的要求,可用于鱼肉中链霉素和双氢链霉素残留的确证检测。
OBJECTIVE To establish a method for the simultaneous determination of streptomycin and dihydrostreptomycin in fish by hydrophilic interaction chromatography-tandem mass spectrometry. Methods Using fish as raw material, the samples were extracted by phosphate buffered saline, purified by solid phase extraction (SPE) column and separated by hydrophilic interaction column. The data were determined by electrospray ionization tandem mass spectrometry in positive ion mode and quantified by external standard method. Results The linearity of streptomycin and dihydrostreptomycin in the range of 2.0 ~ 50μg / L was good. The recoveries of the method were 80.2% ~ 97.1% at the three spiked levels of 10, 20 and 50μg / kg, The relative standard deviation was 3.3% ~ 7.2%. Conclusion The method is simple, rapid, practical and accurate, and the technical indexes meet the requirements of domestic and foreign laws and regulations. It can be used to confirm the streptomycin and dihydrostreptomycin residues in fish meat.