液相色谱-串联质谱法分析海产品中四环素类药物残留

Determination of 4 Tetracyclines Residues in Seafoods by Liquid ChromatographyMass Spectrometry

  • 摘要: 为满足海产品检测中对快速、低检出限分析方法的迫切需要,建立了海产品中四环素类抗生素(四环素、土霉素、金霉素、强力霉素)残留量的测定方法。样品经过2%的高氯酸提取,固相萃取柱净化,以乙腈水三氟乙酸体系为流动相,采用电喷雾离子源以正离子检测方法进行质谱分析。结果显示,样品中4种化合物的定性限(LOD)为:金霉素0.008 mg•kg-1,其他3种化合物均为0.002 mg•kg-1;定量限(LOQ)为:金霉素0.02 mg•kg-1,其他3种化合物均为0.006 mg•kg-1;线性范围为0.01~0.1 mg•L-1, 相关系数大于0.995。从0.05、0.08、0.1 mg•kg-1 3个添加浓度检测结果可见,平均回收率为50.2%~91.2%,RSD为4.0%~9.2%,可以满足海产品中四环素类抗生素残留量的监测要求。

     

    Abstract: A method for the determination of 4 tetracyclines (tetracycline, oxytetracycline,doxycycline, chlortetracycline) residues in seafood was developed. Sample was extracted with 2% perchloric acid, purified by a solid-phase extraction procedure. Then the reconstituted sample solution was analyzed by UPLC-MS/MS in ESI position mode using the mobile phase with trifluoroacetic acid(TFA)/water and acetonitritrile. The detection limits of chlortetracycline is 0.008 mg•kg-1, the others are 0.002 mg•kg-1. The quantification limit of chlortetracycline is 0.02 mg•kg-1, the others are 0.006 mg•kg-1. Range of the calibration curve 4 tetracycline is 0.01-0.1 mg•L-1, and RSD is more than 0.995. The average recoveries from spiked sample at 3 concentrations of 0.05, 0.08, 0.1 mg•kg-1 range from 50.2% to 91.2%, and RSD is 4.0%-9.2%。

     

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