Quantification of ultra-trace organolead species in environmental water by inductively coupled plasma mass spectrometry with online solid-phase extraction and high performance liquid chromatographic separation.

Quantification of organolead compounds in environmental water is an essential task considering much higher toxicity and bioavailability of organolead species than inorganic plumbic ions. However, the speciation of ultra-trace organolead compounds at sub ng L levels is challengeable for current instruments incorporating high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) and even offline enrichment that offer detection limits around several to tens of ng L. In this paper, an online solid-phase extraction (SPE) coupled HPLC-ICP-MS method was developed for speciation analysis of trace lead in water. Graphene oxide bounded silica particles (GO@SiO) was utilized as the SPE adsorbent because of its superior performance over graphene bounded silica particles and commercial C packing particles. High enrichment factors (1603 for TML and 1376 for TEL) were obtained when lead species in 10 mL sample was adsorbed by 1 mM sodium dodecyl benzene sulfonate (SDBS) preconditioned GO@SiO at 10 mL min and then eluted by 5 μL of 5 mM SDBS. Because of the highly efficient preconcentration, detection limits were downscaled to be 0.018 for TML and 0.023 ng L for TEL with relative standard deviations below 5%. Additionally, the proposed method also yielded rapid separation of Pb(II), TML and TEL (8 min) by using green mobile phases (aqueous solutions of 5 mM sodium 1-pentanesulfonate at pH 2.5 with/without 4 mM tetrabutylammounium hydroxide). Upon successful application to fresh water, TML and TEL were only presented in the river water whereas Pb(II) was only existed in the tap water, along with accuracy validation by good spiked recoveries (93-106%).