固相萃取-高效液相色谱串联质谱法测定水中58种抗生素方法研究

Study on determination of 58 antibiotics in water by solid-phase extraction with high performance liquid chromatography-tandem mass spectrometry

建立了固相萃取-高效液相色谱串联质谱法测定水中58种抗生素的分析方法。水样经过全自动固相萃取仪富集,以HLB柱为萃取柱,4mL甲醇和4mL 0.1%甲酸甲醇为洗脱剂,用高效液相色谱串联质谱仪分析定量。该方法在1.0~100μg·L^(-1)范围内线性良好,相关系数均大于0.995,58种抗生素的纯水加标回收率为72.4~115%,地表水加标回收率为68.2~97.6%,地下水加标回收率为71.7~112%,污水处理厂出厂水加标回收率为62.5~96.7%,相对标准偏差均小于15%,检出限为0.02~0.8ng·L^(-1),该方法简单实用、准确可靠,可用于水中58种抗生素的高通量同时测定。

A solid-phase extraction high-performance liquid chromatography tandem mass spectrometry method was established for the determination of 58 antibiotics in water.The water sample was enriched by a fully automated solid-phase extraction instrument,using an HLB column as the extraction column and 4 mL methanol and 4 mL 0.1%formic acid methanol as eluents.Quantitative analysis was performed using high-performance liquid chromatography tandem mass spectrometry.The method had good linearity in the range of 1.0~100μg·L^(-1),and the correlation coefficients were all greater than 0.995,the recoveries of 58 antibiotics were 72.4~115%in pure water,68.2~97.6%in surface water and 71.7~112%in groundwater and the standard recovery rate of water from sewage treatment plant was 62.5~96.7%.The relative standard deviation was less than 15%,and the detection limit was 0.02~0.8ng·L^(-1).This method is simple,practical,accurate,and reliable,and can be used for the high-throughput simultaneous determination of 58 antibiotics in water.