Elsevier

Food Chemistry

Volume 215, 15 January 2017, Pages 447-453
Food Chemistry

Analytical Methods
Simultaneous preconcentrations of Co2+, Cr6+, Hg2+ and Pb2+ ions by Bacillus altitudinis immobilized nanodiamond prior to their determinations in food samples by ICP-OES

https://doi.org/10.1016/j.foodchem.2016.07.055Get rights and content

Highlights

  • B. altitudinis immobilized nanodiamond was used for preconcentration of Co2+, Cr6+, Hg2+ and Pb2+.

  • The analytical parameters were optimized for quantitative recoveries of analytes.

  • The method was validated through the analysis of certified reference materials.

  • The method was applied to food samples to determine analyte concentrations.

Abstract

A novel solid phase extraction method was developed for simultaneous preconcentration-separation of Co2+, Cr6+, Hg2+ and Pb2+ ions prior to their determinations in food samples by ICP-OES. Thermophilic Bacillus altitudinis immobilized nanodiamond was used as a new biosorbent. SEM and FT-IR analysis were studied to characterize the biosorbent. The optimum pH values of quantitative biosorption for Co2+, Cr6+, Hg2+ and Pb2+ were found to be 5.0, 6.0, 6.0 and 6.0, respectively. A flow rate of 3.0 mL min−1 was selected as optimum for all metal ions. 5 mL of 1 mol/L HCl was used as eluent. Preconcentration factor was achieved as 80. LODs were calculated as 0.071, 0.023, 0.016 and 0.034 ng mL−1, respectively for Hg2+, Co2+, Cr6+ and Pb2+. The biosorption capacities were calculated for Co2+, Cr6+, Hg2+ and Pb2+ as 26.4, 30.4, 19.5, and 35.2 mg/g, respectively. The developed method was successfully applied to food samples to determine analyte concentrations.

Introduction

The pollution of the environment by harmful heavy metal ions has attracted great attention over last few years. There are more than 20 heavy metals, but some of them, such as cadmium (Cd), lead (Pb) and mercury (Hg) are highly toxic and can cause damaging effects even at very low concentrations on living system (Kocaoba & Arısoy, 2011). Cobalt (Co) and chromium (Cr) are toxic when used in large amounts and long period exposure to both metals one of the reasons behind toxicity (Costa and Klein, 2006, Ozdemir et al., 2012). Direct determination of metal ions in food, soil and water samples by instrumental analysis is often difficult because of low concentration of trace metal ions and presence of interferences. Therefore, a separation and preconcentration technique is often required before determination (Mirabi et al., 2015, Ozdemir et al., 2016).

Many sample pretreatment methods (e.g. solid-phase extraction, liquid-liquid extraction, precipitation, ion exchange and cloud-point extraction) are usable for separation and preconcentration of trace metals in different samples (Afkhami et al., 2006, Chen et al., 1997, Okumus et al., 2015). Among these methods, solid-phase extraction (SPE) procedures are considered superior to other procedures for their simplicity, better efficiency and a higher preconcentration factor (Ozdemir, Okumus, Dundar, & Kilinc, 2013).

New solid materials have recently emerged as alternatives to traditional SPE sorbents with the aim of obtaining a more selective preconcentration of the target metal ions (Madrakian, Zadpour, Ahmadi, & Afkhami, 2015). The use of microbial biomass and metallic nanoparticles for the preconcentration and separation of heavy metals at trace levels are popular due to the good adsorption properties such as high surface area, high adsorption capacity and low temperature modification (Hassanpoor et al., 2015, Kilinc et al., 2013a).

Nanodiamond has excellent mechanical properties, tunable surface structures and high surface areas. It is also non-toxic the surface area of nanodiamond is about 450 m2 g−1, which makes it potential superior adsorbents (Cicala et al., 2014, Huang and Chang, 2004).

The present work aimed the use of thermophilic Bacillus altitudinis immobilized nanodiamond as a novel biosorbent for the separation and preconcentration of Co2+, Cr6+, Hg2+ and Pb2+. Immobilized biosorbent was characterized by FT-IR and SEM. Various influencing parameters such as, pH value, amount of nanoparticles, amount of bacterial biomass, flow rate, volume of sample solution, and effect of major ions on the preconcentration of the tested metal ions were studied. The recommended method was validated through analysis of the certified and standard reference materials (DORM-2, DOLT-3, SRM 1643e, NCZ ZC73014, NCS DC73351). It was successfully utilized to the determination of cobalt, chromium, mercury and lead in water and food samples.

Section snippets

Instrumentation

Concentrations of cobalt, chromium, mercury and lead were measured by ICP-OES at 228.616, 267.716, 194.168 and 220.353 nm, respectively (Perkin Elmer Optima™ 2100 DV, PerkinElmer, Inc., Shelton, CT, USA) under the instrumental operating conditions recommended by producer. pH of the solutions were measured by Mettler Toledo MPC 227 (Polaris Parkway, Columbus, OH, USA) digital pH meter. Filtration column (1.0 cm × 10.0 cm), equipped with polypropylene frites was used in SPE experiments. Peristaltic

Results and discussion

Surface morphologies of nanodiamond and B. altitudinis immobilized nanodiamond were investigated by SEM. Results were presented in Fig. 1a and b. It could be possible to discuss that microstructure of nanodiamond protected after immobilization of B. altitudinis. The major advantage of B. altitudinis immobilization was to increase the surface functionalities through the affinity to metal ions. Surface functionalities of nanodiamond and B. altitudinis immobilized nanodiamond were investigated by

Conclusion

A novel solid phase extraction method was developed for the preconcentration of Co2+, Cr6+, Hg2+ and Pb2+. Bacillus altitudinis immobilized on nanodiamond was firstly used as biosorbent for this purpose. The method was accurate through the analysis of certified and standard reference materials. Preconcentration factor was achieved as 80. RSDs were found lower than 5%. The results showed that the immobilized biosorbent column could be reused at least 30 cycles of biosorption and desorption with

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