Determination of Macrolide Antibiotics in Water by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Quadrupole Linear Ion Trap Mass Spectrometry
Five macrolide antibiotics detection methods,including azithromycin,lincomycin,clindamycin,erythromycin and tilmicosin,in water were established by using solid phase extraction-ultra performance liquid chromatography-triple quadrupole linear ion trap mass spectrometry(SPE-UPLC-QTRAP MS).The macrolide antibiotics in water samples were enriched with HLB solid phase extraction column at pH=10,then separated by Kinetex F5 chromatographic column,and eluted in gradient with 0.1%formic acid aqueous solution and 0.1%formic acid acetonitrile,respectively.The water samples were detected by multiple reaction monitoring(MRM)-information-dependent acquisition(IDA)-enhancer ion(EPI)scan mode using electrospray positive ion source(ESI+),and the EPI library and MRM were employed for the rapid confirmation and quantitative determination.The results showed that good linearity for five macrolide antibiotics and the correlation coefficient was higher than 0.9992.The limits of detection were 0.01-0.30 μg·L-1,and the limits of quantification were 0.10-0.50 μg·L-1.The recoveries of spiked water samples with three different concentrations were 71.60%-111.05%,and the relative standard deviations(RSD)were within 10%.The purity of EPI spectrum library was greater than 90%.This method combined traditional MRM scanning mode with EPI spectrum library retrieval,and achieved simultaneous qualitative and quantitative analysis.It can provide an important reference for the laboratory on deterministic and quantitative detection of unknown substance.
Macrolide antibioticsSolid-phase extractionLinear ion trapLiquid chromatograph-mass spectrometerResidual detection