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建立了不使用离子对试剂,液质联用技术检测鳗鱼中链霉素和双氢链霉素残留量的检测方法。样品经三氯乙酸溶液提取,碱性氧化铝快速净化,弱阳离子交换柱固相萃取,CAPCELL PAK ST柱分离。链霉素和双氢链霉素检出限为1.5μg/kg,在10.0~500 ng/m L质量浓度范围内链霉素和双氢链霉素呈线性相关,相关系数为0.9999和0.9994,回收率在78.3%~105.9%之间,相对标准偏差在3.1%~6.6%之间。方法采用碱性氧化铝基质分散固相萃取,除去样液中油脂同时也降低样液中酸的浓度,进而降低固相萃取上样液中碱金属离子强度,提高了链霉素和双氢链霉素残留检测的绝对回收率。
The method for detecting streptomycin and dihydrostreptomycin residues in eels without ion pair reagent and liquid chromatography-mass spectrometry (LC-MS / MS) was established. The samples were extracted with trichloroacetic acid solution, rapidly purified with basic alumina, and subjected to weak cation exchange column solid phase extraction (CAPCELL PAK ST column). The detection limit of streptomycin and dihydrostreptomycin was 1.5μg / kg. There was a linear correlation between streptomycin and dihydrostreptomycin in the concentration range of 10.0-500 ng / m L with correlation coefficients of 0.9999 and 0.9994. The recoveries ranged from 78.3% to 105.9% with relative standard deviations between 3.1% and 6.6%. Methods Al Base Alumina Matrix Dispersive Solid Phase Extraction was used to remove the oil from the sample solution and also to reduce the acid concentration in the sample solution, thereby reducing the intensity of alkali metal ions in the solid phase extraction sample and increasing the concentration of streptomycin and dihydrogen chains Absolute recovery of mycophenolate residues.