研究了鱼肉中氯霉素和甲砜霉素残留量的气相色谱测定方法。鱼肉中的待测物用乙酸乙酯提取,浓缩至干,溶于水,用正己烷脱脂,水层过 C18小柱,用甲醇洗脱后,用 N, O - 双(三甲基硅烷基)三氟乙酰胺( BSTFA)+ 1% (φ )三甲基氯硅烷( TMCS)衍生,加入甲苯并用水灭活衍生过程。用外标法定量。当添加水平( w)为 5× 10- 9~ 20× 10- 9时,回收率为 80%~ 108%。相对标准偏差为 4.5%~ 11%;线性相关系数 r>0.997。%A gas chromatographic (GC) method is described for the determination of chloramphenicol(CAP) and thiamphenicol(TAP) residues in fish tissues. Samples were extracted with ethyl acetate, and evaporated to dryness. The residues were dissolved in water, defatted with hexane, and passed through a C18 SPE column. The C18 SPE column was eluted with MeOH . The eluate was derivatized with N,O -bis(trimethylsilanyl)trifluoroacetamide(BSTFA)+ 1% trimethylchlorosilane(TMCS). After derivatization, toluene was added to sample, followed by water, to quench the derivatization process. The quantitative determination was performed with an external standard method. The relative standard deviations were 4.5% ~ 11% , and the recoveries were 80% ~ 108% . The correlation coefficient r>0.997.
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