采用磁性多壁碳纳米管-超高效液相色谱/质谱/质谱(UPLC/MS/MS)技术测定水样中23种抗生素残留量。水样基质中的23种抗生素药物先采用磁性多壁碳纳米管(MWCNTs)富集和净化，再用5%的氨水甲醇溶液脱附，23种化合物以CORTECSTM C18+色谱柱分离，甲醇和0.1%的甲酸水溶液作为流动相，采用电喷雾正离子(ESI+)和多反应监测模式(MRM)分析，外标法定量。23种抗生素在0.5~50 μg/L的浓度范围内线性相关系数均大于0.99，检出限为0.01 μg/L，定量限为0.03 μg/L。在0.05、0.5、10 μg/L不同浓度水平下，23种抗生素的平均回收率在87.5%~105.8%之间，相对标准偏差在0.3%~4.2%之间。由于该技术简便、快速、灵敏度高，适用于水中23种抗生素残留的快速测定。
A method was established for determining 23 antibiotics residues in water samples by magnetic multiwalled carbon nanotubes and ultra performance liquid chromatography-tandem mass spectrometry (UPLC/MS/MS). The 23 antibiotics in water samples were first enriched and cleaned up by magnetic multiwalled carbon nanotubes, and then eluted with ammonium hy-droxide-methanol (5:95, v/v). The target antibiotics were separated by Waters CORTECSTM C18+ column using methanol and 0.1% formate in water as mobile phases. The analytes were detected by positive electrospray ionization with multiple reaction monitoring. External standard method was used to determine the quantity. In the linear range of 0.5~50 μg/L, the correlation coefficients of 23 antibiotics were greater than 0.99, the limit of detection (LOD) was 0.01 μg/L, and the limit of quantitation (LOQ) was 0.03 μg/L. The mean recoveries at the three spiked levels of 0.05, 0.5, 10 μg/L were 87.5%~105.8%. The relative standard deviation (RSD) was 0.3%~4.2%. The simplicity, sensitivity and good precision of the method made it be well suitable for quick determination of the 23 antibiotics residues in water samples.
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