超高效液相色谱串联质谱测定中水中喹诺酮类抗生素

Determination of Quinolones Antibiotics in Reclaimed Water by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometer

建立了检测中水中14种喹诺酮类抗生素残留的超高效液相色谱串联质谱(UPLCMS/MS)方法。水样通过HLB固相萃取小柱富集后,经C18色谱柱分离,运用乙腈-0.2%甲酸的10 mmol/L甲酸铵溶液进行梯度洗脱,质谱仪检测。采用电喷雾正模式电离(ESI+),多反应监测(MRM)模式进行检测,外标法定量。在1~100 ng/m L的线性范围内,各物质的线性关系良好,线性相关系数均≥0.991,方法的检出限为0.2~1.0 ng/L,定量限为0.5~2.0 ng/L,回收率稳定,RSD≤16%。该方法方便、准确,适用于中水中抗生素的痕量分析。

A method for the determination of 14 quinolones antibiotics residues in reclaimed water by ultra performance liquid chromatography （UPLC-MS/MS） was developed. Water samples are firstly enriched by HLB solid phase extraction, then separated by C18 column and eluted with acetonitrile and 10 mmol/L ammonium formate solution with O. 2% formic acid included, the mass spectrometer is used for finally detection. The samples were ionized by positive electrospray ionization mode （ESI ＋ ）, detected by multiple reaction mode （ MRM）, and quantified by external standard method. In the range of 1 - 100 ng/mL, the regression equation of the antibiotics showed good liner relationship, and the linear correlation coefficients were no less than 0.991. The limits of detection and quantification were 0.2 - 1.0 ng/L and 0.5 - 2.0 ng/L respectively. As a result, the recoveries were stable, and the RSDs were less than 16%. The method is convenient and accurate, and could be applied to the trace analysis of antibiotics in reclaimed water.