Rapid Speciation of Lead in Human Blood and Urine Samples Based on MWCNTs@DMP by Dispersive Ionic Liquid-Suspension-Micro-Solid Phase Extraction.

An efficient sorbent based on 2,3-dimercapto-1-propanol immobilized on multi-wall carbon nanotubes (MWCNTs@DMP) was developed for separation/speciation of organic and inorganic lead (alkyl-Pb, Pb2+) in human blood, urine, and water samples by dispersive ionic liquid-suspension-micro-solid phase extraction (DIL-S-μ-SPE). By procedure, the MWCNTs@DMP as solid phase, acetone, and ionic liquid (IL, [HMIM][PF6]) were mixed and injected to 10 mL of the liquid phase at pH = 6.5. After shaking, the Pb(II) was extracted in MWCNTs@DMP and settled down in a conical tube with IL by centrifuging (Pb2+→: SH-SiO2@CNTs). The lead (Pb2+) was back-extracted from sorbent/IL in acidic pH and measured by atom trap atomic absorption spectrometry (AT-AAS). In addition, the organic lead (R-Pb, alkyl lead) converted to Pb(II) and total lead (T-Pb) was determined in the same conditions by UV radiation in 95 °C. Under the optimal conditions, the linear range (9.5-480 μg L-1), LOD (3.2 μg L-1), and enrichment factor (10.4) were obtained (RSD < 5%). The adsorption capacity of the MWCNTs@DMP and MWCNTs was achieved as 191.6 mg g-1 and 25.8 mg g-1, respectively. The method was validated by standard reference materials (SRM 1643d, SRM 955, and SRM 2668), ET-AAS, and ICP-MS analysis in real samples. Graphical abstract.