饮用水中12种抗生素残留的固相萃取-超高效液相色谱-串联四极杆飞行时间质谱快速测定法

Rapid determination of 12 antibiotic residues in drinking water by solid phase extraction and ultraperformance liquid chromatography coupled to time of flight mass spectrometry

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 develop a rapid determination method based on solid phase extraction and ultra-performance liquid chromatography coupled to time of flight mass spectrometry to determine twelve kinds of antibiotic residues in drinking water.Methods The water samples were passed through HLB cartridges in order to extract and purify,and the target compounds were separated by a ACQUITY UPLC BEH C18 column（100 mm×2.1 mm,1.7 μm）,using acetonitrile and 0.1% formic acid solution as the mobile phase by gradient elution.The detection was under positive electrospray ionization（ESI＋） mode,The quantitative analysis was carried out by extracting the peak area with accurate mass. The confirmatory analysis of the target compounds was performed with the qualitative fragments. Results In the linear range of 0.1-500 ng/L,the regression equation of the twelve antibiotics showed good liner relationship（r〉0.99）. The detection limits of the method were 0.018-6.0 ng/L,the lower limits of quantification were 0.06-20 ng/L.The average recovery rates were 65.4%-84.7%,and the RSDs were 4.5%-11.7%.Conclusion The method is simple,rapid,accurate,sensitive and applicable to the rapid screening of antibiotic residues in drinking water.