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Efficiency of different green shaking extraction methods for the preconcentration of trace quantity of mercury in artificial saliva extract of snuff products: impact on adult consumers

Asma Akhtar, Tasneem Gul Kazi, Hassan Imran Afridi, Jameel Ahmed Baig, Syed Ghulam Musharraf, and Mohammad Balal Arain

National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro, Pakistan



Received: 14 August 2020  Accepted: 28 January 2021


The present study is based on developing a dual-step ultrasonically modified cloud point extraction (DsUm-CPE) method for enrichment of mercury (Hg) in artificial saliva extract (ASE) of the numerous snuff products (dry and moist snuff, having green, brown and black in colors). This method relies on the complexation of Hg with ammonium O, O-diethyldithiophosphate, followed by the entrapped in nonionic surfactant (Triton X-114) prior to analysis by cold vapor atomic absorption spectrometry (CVAAS). The dispersion of hydrophobic complex in micellar phase was carried out by ultrasound energy, in addition other shaking method, vortex mixer was also applied for comparison purposes, vortex shaking method was also used. Several variables of developed methods, such as complexing agent, Triton X-114, dispersion modes (sonication/vortex shaking), equilibrium temperature, centrifugation time and concentration of back extraction reagent, have been studied. The detection and quantification limit under the optimum conditions were attained as 0.004 and 0.014 µg L−1, respectively. The accuracy for the analysis of total Hg was checked by certified samples of Virginia tobacco leaves (ICHTJ-cta-VTL-2) and both biological samples. The obtained values of all three certified samples have insignificant difference (p > 0.05) among their certified and experimental values. The resulted statistics specified that dry snuff has about fourfold higher contents of Hg as compared to moist snuff, whereas the biological samples of male subject (25 to 60 years) sniffing moist and dry snuff were also analyzed to assess the Hg exposure through their consumption. The biological samples of snuff consumers have about twofold higher concentration of Hg as compared to referents.

Keywords: Smokeless tobacco products; Moist and dry snuff; Artificial saliva extract; Mercury; Ultrasound energy; Cloud point extraction

Full paper is available at

DOI: 10.1007/s11696-021-01545-7


Chemical Papers 75 (7) 3005–3015 (2021)

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