固相萃取/超高效液相色谱—串联质谱法测定水中7种大环内酯类抗生素

建立了测定水中7种大环内酯类抗生素的固相萃取/超高效液相色谱—串联质谱分析方法。将水样经固相萃取后进样,经ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7μm)分离,采用三重四级杆串联质谱法在多反应监测模式进行检测,外标法定量。方法的线性范围为2~100μg/L,线性相关系数均大于0.995,样品100倍浓缩后,检出限低至0.004~0.009μg/L;在20~1 000 ng/L范围内,2个不同浓度加标样品的回收率为80.5%~92.5%,相对标准偏差为3.6%~11%。该方法能够满足国家新型污染物治理的需要,方法高效准确、灵敏度高。

An analytical method for the determination of seven macrolide antibiotics in water by solid-phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry was established. The water samples were injected after solid-phase extraction,separated by ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7 μm),and detected by triple quadrupole tandem mass spectrometry in multiple reaction monitoring(MRM)mode,and quantified by external standard method. The linear range of the method was 2-100 μg/L,and the linear correlation coefficients were all greater than 0.995. After 100-fold concentration of the sample,the detection limit was as low as0.004-0.009 μg/L;in the range of 20-1 000 ng/L,the recoveries of the samples spiked with medium and low concentrations were 80.5%-92.5%,respectively;the relative standard deviations(RSD)were 3.6%-11%. The method can meet the needs of national new pollutant control,and the method is efficient,accurate and sensitive.