Homogeneous liquid–liquid microextraction based on liquid nitrogen-induced phase separation followed by GFAAS for sensitive extraction and determination of lead in lead-adulterated opium and refined opium

Abstract

Herein, we developed a novel homogeneous liquid–liquid microextraction based on liquid nitrogen-induced phase separation (HLLME-LNPS) for the extraction and determination of lead (Pb) in Pb-adulterated opium and refined opium by GFAAS analysis. In this procedure, first, 400 μl of acetonitrile (extractant) containing 7.0 μl of diethyl dithiophosphoric acid (DDTP) is injected into a sample solution and a homogeneous solution is formed. Subsequently, the homogeneous mixture is cooled using liquid nitrogen for 16 seconds. By this process, due to the difference in the freezing points of the organic and aqueous phases, the homogeneous state is broken and the Pb-DDTP species are extracted into the liquid organic phase collected on top of the frozen aqueous phase. The introduced method exhibited a good linearity with a coefficient of determination (r²) of 0.9988 and an acceptable linear range of 0.6–100 μg l⁻¹. Accordingly, the detection limit was 0.2 μg l⁻¹ (S/N = 3) for Pb ions, and a high enrichment factor was obtained. The proposed method was successfully utilized to determine trace levels of Pb in opium samples. The results of the sample analysis showed that 65% of the opium samples and 85% of the refined opium samples had much higher than expected levels of contaminating Pb, and this contamination poses a serious threat to drug users.