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目的建立了饮用水中12种抗生素残留的固相萃取(SPE)-超高效液相色谱-串联四极杆飞行时间质谱(UPLCQTOF)快速测定法。方法水样经过HLB小柱浓缩萃取之后以ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm)为分析柱,以乙腈-0.1%甲酸溶液为流动相进行梯度洗脱;质谱采用高分辨质谱、正离子模式,以精确质量数和二级特征离子定性,以准分子离子峰面积定量。结果在0.1~500 ng/L的线性范围内,所得12种抗生素的回归方程均呈较好的线性关系,r>0.99;该方法的检出限为0.018~6.0 ng/L,定量下限为0.06~20 ng/L,回收率为65.4%~84.7%,RSD为4.5%~11.7%。结论该法操作简单、快速、准确、灵敏、适用于饮用水中抗生素的快速筛查测定。
Objective To establish a rapid solid phase extraction (SPE) - ultra performance liquid chromatography-tandem quadrupole time-of-flight mass spectrometry (UPLCQTOF) rapid determination method for 12 antibiotic residues in drinking water. Methods The aqueous samples were concentrated by HLB cartridge and eluted with ACQUITY UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with acetonitrile-0.1% formic acid as mobile phase. Mass spectrometry, positive ion mode, with accurate mass number and secondary characteristic ion qualitative, quasi molecular ion peak area. Results The regression equation of the 12 antibiotics showed a good linearity within the linear range of 0.1-500 ng / L with r> 0.99. The detection limit of this method was 0.018-6.0 ng / L, and the lower limit of quantification was 0.06 ~ 20 ng / L, the recoveries were 65.4% ~ 84.7% and the RSD was 4.5% ~ 11.7%. Conclusion The method is simple, rapid, accurate and sensitive and is suitable for the rapid screening of antibiotics in drinking water.