Development and application of ultra performance liquid chromatography-electrospray ionization tandem triple quadrupole mass spectrometry for determination of seven microcystins in water samples

摘要

In the present work,an ultra performance liquid chromatography(UPLC)-electrospray ionization tandem triple quadrupole/mass spectrometry(ESI-MS/MS)method was developed in selected reaction monitoring(SRM)mode to determine the amounts of seven/microcystin variants(MCYST-RR,-YR,-LR,-LA,-LY,-LW,-LF)in water samples.Solid phase extraction(SPE)or porous filter was used for sample cleaning-up and analyte enrichment.A C18 column enabled separation of 7 microcystins within 10 min.Translation reaction ions including 995.6>134.9(RR),1045.8>135.1(YR),910.9>375.7(LA),1002.3>375.6(LY),520.1>135.0(LR),1025.8>891.7(LW),986.8>852.6(LF)were set as quantitative ions and the enkephalin was the internal standard.Upon method validation,the limits of detection(LODs)and limits of quantification(LOQs)were found to be 0.06 mu gL~(-1)and 0.2mu gL~(-1)(injection volume of 10 mu L),respectively,for all seven microcystin variants.The correlation coefficients were larger than 0.994 in all linear ranges and recoveries were in the range of 66.24-99.22%.The developed approach was highly sensitive and easy to perform.It generated accurate quantitative results for the analysis of microcystins in environmental water samples with a wide concentration range.The results showed that MC-RR and MC-LR widely existed in polluted water,while MC-LA and MC-LY were detected sporadically.