Adsorption and determination of Lead in water and human urine samples based on Zn2(BDC)2(DABCO) MOF as polycaprolactone nanocomposite by suspension micro solid phase extraction coupled to UV–VIS spectroscopy

Volume 4, Issue 03, Pages 5-20, Sep 2021 *** Field: Analytical Environmental Chemistry

  • Negar Motakef kazemi, (Corresponding Author) Department of Medical Nanotechnology, Faculty of Advanced Sciences and Technology, Tehran Medical Sciences, Islamic Azad University, Tehran, Iran
  • Masomeh Odar Odar Department of Nanochemistry, Faculty of Pharmaceutical Chemistry, Tehran Medical Sciences, Islamic Azad University, Tehran, Iran
Keywords: Lead, Metal organic framework, Polycaprolactone, Nanocomposite, Adsorption, Suspension-micro-solid phase extraction procedure


Today, the safety of water resource is the most important challenges which was reported by health and environment organizations. Water pollution can be created by hazardous contaminants of environmental pollutions. Lead as a heavy metal has carcinogenic effects in humans. Metal organic framework (MOF) is a highly porous material with different application. The Zn2(BDC)2(DABCO) is a good candidate of MOF based on zinc metal (Zn-MOF) with potential adsorption/extraction. In this work, Zn2(BDC)2(DABCO) MOF as polycaprolactone (PCL) nanocomposite were applied for lead adsorption/extraction from 50 mL of aqueous solution by ultra-assisted dispersive suspension-micro-solid phase extraction procedure (USA-S- µ-SPE) at pH=8. The samples were characterized by the FTIR, the XRD analysis, the FE-SEM and the BET surface area. The effect of parameters was investigated on lead absorption before determined by UV–VIS spectroscopy. The linear range, the detection limit (LOD) and enrichment factor of adsorbent were obtained 0.05-1 mg L-1, 0.25 μg L-1 and 48.7, respectively (= 0.9992, RSD%=3.65). The absorption capacity of Zn2(BDC)2(DABCO) MOF for 50 mg L-1 of standard lead solution were obtained 133.8 mg g-1 for 0.25 g of adsorbent. The results indicate that this nanocomposite can have a good potential to develop different adsorbents.



P.B. Tchounwou, C.G. Yedjou, A.K. Patlolla, D.J. Sutton, Heavy metals toxicity and the environment, EXS J., 101 (2012) 133–164.

A. Latif Wani, A. Ara, J. Ahmad Usmani, Lead toxicity: a review, Interdiscip. Toxicol., 8 (2015) 55–64.

G. Flora, D. Gupta, A. Tiwari, Toxicity of lead: a review with recent updates, Interdiscip. Toxicol., 5 (2012) 47-58.

M. Kosnett, Heavy metal intoxication and chelators, Basic and clinical pharmacology, 10th ed, New York: McGraw-Hill, (2007) 945-957.

Agency for Toxic Substances and Disease Registry (ATSDR), Toxicological profile for Lead, Atlanta, GA: U.S. Department of Health and Human Services, Public Health Service, 2019.

R. Arora, Adsorption of heavy metals–a review, Mater. Today, 18 (2019) 4745-4750.

J. Yang, B. Hou, J. Wang, B. Tian, J. Bi, N. Wang, X. Li, X. Huang, Nanomaterials for the removal of heavy metals from wastewater, Nanomater., 9 (2019) 424.

M.J. González-Muˇnoz, M.A. Rodríguez, S. Luque, J.R. Àlvarez, Recovery of heavy metals from metal industry wastewaters by chemical precipitation and nanofiltration, Desalination, 200 (2006) 742–744.

MY. Vilensky, B. Berkowitz, A. Warshawsky, In-situ remediation of groundwater contaminated by heavy- and transition-metal ions by selective ion-exchange methods, Environ. Sci. Technol., 36 (2002) 1851–1855.

M.G. Khedr, Nanofiltration and low energy reverse osmosis for rejection of radioactive isotopes and heavy metal cations from drinking water sources, Desalination Water Treat., 2 (2009) 342–350.

S.B. Wang, H.W. Wu, Environmental-benign utilization of fly ash as low-cost adsorbents, J. Hazard. Mater., 136 (2006) 482–501.

M. Odar, N. Motakef Kazemi, Nanohydroxyapatite and its polycaprolactone nanocomposite for lead sorbent from aqueous solution, Nanomed. Res. J., (2020) Accepted.

A. Alghamdi, AB. Al-Odayni, W. Sharaf Saeed, A. Al-Kahtani, FA. Alharthi, T. Aouak, Efficient adsorption of lead (II) from aqueous phase solutions using polypyrrole-based activated carbon, Materials, 12 (2019) 2020.

B. Feist, M. Pilch, J. Nycz, Graphene oxide chemically modified with 5-amino-1, 10-phenanthroline as sorbent for separation and preconcentration of trace amount of lead (II), Microchim. Acta, 186 (2019) 91.

M.R. Karim, M.O. Aijaz, N.H. Alharth, H.F. Alharbi, F.S. Al-Mubaddel, M.R. Awual, Composite nanofibers membranes of poly (vinyl alcohol)/chitosan for selective lead (II) and cadmium (II) ions removal from wastewater, Ecotoxicol. Environ. Safe., 169 (2019) 479-486.

E. Kazemi, S. Dadfarnia, A.M. Haji Shabani, P.S. Hashemi, Synthesis of 2-mercaptobenzothiazole/magnetic nanoparticles modified multi-walled carbon nanotubes for simultaneous solid-phase microextraction of cadmium and lead, Int. J. Environ. Aanal. Chem., 97 (2017) 743-755.

M. Mashkani, A. Mehdinia, A. Jabbari, Y. Bide, M.R. Nabid, Preconcentration and extraction of lead ions in vegetable and water samples by N-doped carbon quantum dot conjugated with Fe3O4 as a green and facial adsorbent, Food Chem., 239 (2018) 1019-1026.

H. Shirkhanloo, S.D. Ahranjani, A lead analysis based on amine functionalized bimodal mesoporous silica nanoparticles in human biological samples by ultrasound assisted-ionic liquid trap-micro solid phase extraction, J. pharm. Biomed. Anal., 157 (2018) 1-9.

F. Ataei, D. Dorranian, N. Motakef-Kazemi, Bismuth-based metal–organic framework prepared by pulsed laser ablation method in liquid, J. Theor. Appl. Phys., 14 (2020) 1–8.

N. Motakef-Kazemi, M. Rashidian, S. Taghizadeh Dabbagh, M. Yaqoubi, Synthesis and characterization of bismuth oxide nanoparticle by thermal decomposition of bismuth-based MOF and evaluation of its nanocomposite, Iran. J. Chem. Chem. Eng., 40 (2021) 11-19.

F. Ataei, D. Dorranian, N. Motakef-Kazemi, Synthesis of MOF-5 nanostructures by laser ablation method in liquid and evaluation of its properties, J. Mater. Sci.: Mater. Electron., 32 (2021) 3819–3833.

B. Miri, N. Motakef-Kazemi, S.A. Shojaosadati, A. Morsali, Application of a nanoporous metal organic framework based on iron carboxylate as drug delivery system, Iran. J. Pharm. Res.,17 (2018) 1164–1171.

H. Li, M. Eddaoudi, M. O’Keeffe, O. Yaghi, Design and synthesis of an exceptionally stable and highly porous metal-organic framework, Nature, 402 (1999) 276–279.

S. Hajiashrafi, N. Motakef-Kazemi, Preparation and evaluation of ZnO nanoparticles by thermal decomposition of MOF-5, Heliyon, 5 (2019) e02152.

N. Motakef-Kazemi, S.A. Shojaosadati, A. Morsali, In situ synthesis of a drug-loaded MOF at room temperature, Micropor. Mesopor. Mater., 186 (2014) 73-79.

N. Motakef-Kazemi, S.A. Shojaosadati, A. Morsali, Evaluation of the effect of nanoporous nanorods Zn2(bdc)2(dabco) dimension on ibuprofen loading and release, J. Iran. Chem. Soc., 13 (2016) 1205-1212.

M.R. Mehmandoust, N. Motakef-Kazemi, F. Ashouri, Nitrate adsorption from aqueous solution by metal–organic framework MOF-5, Iran. J. Sci. Technol. A, 43 (2019) 443–449.

N. Motakef-Kazemi, A novel sorbent based on metal–organic framework for mercury separation from human serum samples by ultrasound assisted-ionic liquid-solid phase microextraction, Anal. Methods Environ. Chem. J., 2 (2019) 67-78.

H. Nabipour, B. Soltani, N. Ahmadi Nasab, Gentamicin loaded Zn2(bdc)2(dabco) frameworks as efficient materials for drug delivery and antibacterial activity, J. Inorg. Organomet. Polymer Mater., 28 (2018) 1206–1213.

K. Xie, Y. He, Q. Zhao, J. Shang, Q. Gu, GG. Qiao, PA. Webley, Pd(0) loaded Zn2(azoBDC)2(dabco) as a heterogeneous catalyst, Cryst. Eng. Comm., 19 (2017) 4182-4186.

I. Senkovska, S. Kaskel, High pressure methane adsorption in the metal-organic frameworks Cu3(btc)2, Zn2(bdc)2dabco, and Cr3F(H2O)2O(bdc)3, Micropor. Mesopor. Mat., 112 (2008) 108–115.

A. Schneemann, V. Bon, I. Schwedler, I. Senkovska, S. Kaskel, R.A. Fischer, Flexible metal–organic frameworks, Chem. Soc. Rev., 43 (2014) 6062-6096.

N.S. Behbahani, K. Rostamizadeh, M.R. Yaftian, A. Zamani, H. Ahmadi, Covalently modified magnetite nanoparticles with PEG: Preparation and characterization as nano-adsorbent for removal of lead from wastewater, J. Environ. Health Sci., 12 (2014) 103.

R. Ricco, K. Konstas, MJ. Styles, J.J. Richardson, R. Babarao, K. Suzuki, P. Scopece, P. Falcaro, Lead(II) uptake by aluminium based magnetic framework composites (MFCs) in water, J. Mater. Chem. A, 3 (2015) 19822–19831.

Y. Wang, J. Xie, Y. Wu, H. Gea, Z. Hu, Preparation of a functionalized magnetic metal–organic framework sorbent for the extraction of lead prior to electrothermal atomic absorption spectrometer analysis, J. Mater. Chem. A, 1 (2013) 8782-8789.

J. Shen, N. Wang, Y. Guang Wang, D. Yu, Xk. Ouyang, Efficient adsorption of Pb(II) from aqueous solutions by metal organic framework (Zn-BDC) coated magnetic montmorillonite, Polymers, 10 (2018) 1383.

Y.L.F. Musico, C.M. Santos, M.L.P. Dalida, D.F. Rodrigues, Improved removal of lead(II) from water using a polymer-based graphene oxide nanocomposite, J. Mater. Chem. A, 1 (2013) 3789–3796.

M. Irandoost, M. Pezeshki-Modaress, V. Javanbakht, Removal of lead from aqueous solution with nanofibrous nanocomposite of polycaprolactone adsorbent modified by nanoclay and nanozeolite, J. Water Process Eng., 32 (2019) 100981.

KM. Seema, BB. Mamba, J. Njuguna, RZ. Bakhtizin, AK. Mishra, Removal of lead (II) from aqueous waste using (CD-PCL-TiO2) bio-nanocomposites, Int. J. Biol. Macromol., 109 (2018) 136-142.

H.R. Cadorim, M. Schneider, J. Hinz, F. Luvizon, A.N. Dias, E. Carasek, B. Welz, Effective and high-throughput analytical methodology for the determination of lead and cadmium in water samples by disposable pipette extraction coupled with high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS), Anal. Lett., 52 (2019) 2133-2149.

N. Mouhamed, K. Cheikhou, G.E.M. Rokhy, D.M. Bagha, M.-D.C. Guèye, T. Tzedakis, Determination of lead in water by linear sweep anodic stripping voltammetry (LSASV) at unmodified carbon paste electrode: optimization of operating parameters, Am. J. Anal. Chem., 9 (2018) 171.

H. Shirkhanloo, A. Khaligh, H.Z. Mousavi, A. Rashidi, Graphene oxide-packed micro-column solid-phase extraction combined with flame atomic absorption spectrometry for determination of lead (II) and nickel (II) in water samples, Int. J. Environ. Anal.Chem., 95 (2015) 16-32.

S. Azimi, Z. Es’haghi, A magnetized nanoparticle based solid-phase extraction procedure followed by inductively coupled plasma atomic emission spectrometry to determine arsenic, lead and cadmium in water, milk, Indian rice and red tea, Bull. Environ. Contam. Toxicol., 98 (2017) 830-836.

Y. Huang, S. Lia, J. Chen, X. Zhang, Y. Chen, Adsorption of Pb(II) on mesoporous activated carbons fabricated fromwater hyacinth using H3PO4 activation: Adsorption capacity kinetic and isotherm studies, Appl. Surf. Sci., 293 (2014) 160– 168.

M. Borjigin, C. Eskridge, R. Niamat, B. Strouse, P. Bialk, E.B. Kmiec, Electrospun fiber membranes enable proliferation of genetically modified cells, Int. J. Nanomed., 8 (2013) 855–864.

How to Cite
Motakef kazemi, N., & Odar, M. O. (2021). Adsorption and determination of Lead in water and human urine samples based on Zn2(BDC)2(DABCO) MOF as polycaprolactone nanocomposite by suspension micro solid phase extraction coupled to UV–VIS spectroscopy. Analytical Methods in Environmental Chemistry Journal, 4(03), 5-20.
Original Article