Third Day Poster Session, 17 June 2010 - NanoTR-VI

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Poster Session, Thursday, June 17
Theme F686 - N1123
Modified Iron Oxide Magnetic Nanoparticles as A New Solid Phase Extractor for Separation and
Preconcentration of Pb(II) in Opium and Heroin Samples and its Determination by FAAS
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Mohammad Ali KarimiP P, Abdolhamid Hatefi-MehrjardiP P, UAsghar Askarpour KabirUP P*
1
PDepartment of Chemistry & Nanoscience and Nanotechnology Research Laboratory (NNRL), Payame Noor University (PNU), Sirjan,
78185-347, Iran
Abstract-We exhibit a new extractive preconcentration procedure for the determination of trace amounts of lead in opiate samples. This
extraction method is based on adsorption of dithizone-lead complex on modified iron oxide magnetite nanoparticles. The amounts of lead in five
opium and heroin samples were in the range of 8 to 30 g/g and 3 to 17 ng/g respectively. The effects of various parameters such as pH, volume
of sample and eluent, type and concentration of eluent, sample volume, amount of adsorbent and interfering ions have been studied. Results
showed a good linear range and precision (RSD=4.6 %, n = 5). The performance of purposed method for the analysis of these samples was
tested by spiking lead ion to samples and recovery was investigated.
Lead is a heavy metal commonly exists in the environment.
It can either be an acute or chronic toxin.P PCar exhausts,
contaminated food, industrial emission and soils are the most
important sources of lead exposure. Exposure to any of the
above mentioned sources of lead through ingestion, inhalation,
or dermal contact can cause significant toxicity [1].
Opiate materials are one of hazardous material and not
have any healthy control. Salesmen and smugglers may add
lead to opium during the process of opium preparation to
increase the weight of opium for more benefits. Several
reports have found lead poisoning symptoms in opium
addicted patients, and also there are many non specific
symptoms mimicking lead poisoning in opium addicted
patients. Therefore, it seems evaluation of blood lead level in
opium addicted patients to be important [2-4].
Nanometer-sized materials have used highly in the all
Scientifics because of their special properties [5,6]. we use
magnetite nanoparticles (MNPs) that are superparamagnetite
with high area, as solid phase extractor. In addition, these nano
sized solid phase extractors can separate rapid and completely
from sample solutions with aid of a generally magnate.
Figure 1. Procedure for magnetic solid-phase extraction.
In this study, alumina-coated magnetite nanoparticles
(FeR3ROR4R/AlR2ROR3R NPs) were successfully synthesized and
modified by dithizone (DTZ) with aid of sodium
dodecylsulfate (SDS) in acidic media to form mixed
hemimicelles for the extraction of Pb(II) from standard
samples. Experimental factors affecting the extraction
efficiency were studied. In next step the adsorbed lead ions
was eluted with nitric acid solution (4.0 M) for determination
with flame atomic absorption spectroscopy (FAAS). Then this
method was applied to extraction and preconcentration of
Pb(II) in opium and heroin samples.
The magnetic nanoparticles (MNPs), alumina-coated
magnetic nanoparticles (ACMNPs) and DTZ immobilized on
SDS (abbreviated as DSIACMNs) were characterized by
XRD, SEM, TEM and FT-IR spectroscopy.
That showed the MNPs and ACMNPs are
superparamagnetite, pure FeR3ROR4R with a spinel structure and
the immobilized process did not change its crystal phase,
5.7±3 nm for MNPs and 18.9±2 nm for ACMNPs at sizes,
demonstrate excellent dispersibility and the immobilization
procedure was achieved successfully.
Ten samples of opium and heroin were selected randomly
from the samples seized by Police Department in Sirjan City.
For opium samples treatment, the samples were burnt in
electric burner at 700°C for 30 minutes and afterwards they
were dissolved in a solution of nitric acid/water (1:1). After
one day, the solutions were warmed, filtered, neutralized with
conc. NHR3R and treated according general procedure. For
heroin samples, 0.5 g of each was dissolved in nitric
acid/water (1:2), filtered, neutralized and treated according
general procedure.
In summary, the new adsorbents of DSIACMNPs were
prepared easily and low-costly. These sorbents were
successfully applied for convenient, fast, simple and efficient
enrichment of trace amounts of silver ions from opium and
heroin samples. Magnetic separation in the method shortened
analysis times greatly. Easy regeneration is another property
of ACMNPs, and the experiments have proved that these
ACMNPs can be reused at least 4 times on average without
the obvious decrease of recovery after wash/calcine
procedures. Furthermore, it avoids the time-consuming
column passing (about 1 h in conventional solid phase
extraction method) and filtration operation, and no clean-up
steps were required. We have a high performance in analytical
parameters.
The authors are grateful for the financial support of the
Nanoscience and Nanotechnology Research Laboratory
(NNRL) of Sirjan Payam Noor University for this work.
* Corresponding author: a_askar_kabir@yahoo.com
[1] G. Lochitch, Clin.Biochem. 26, 371 (1993).
[2] B.L. Chia, C. K. Leng, F.P Hsii, M.H. Yap, Y.K.. Lee, Br. Med. J.
1, 354 (1973).
[3] A.D.Beattie, P.J. Mullin, R.H. Baxter, M.R. Moore. Scott. Med. J.
24, 318 (1979).
[4] E.J .Fitzsimons, J.H. Dagg. Br. J. Clin. Pract. 36, 284 (1982).
[5] G.P. Rao, C. Lu, F.S. Su, Sep. Purif. Technol. 58, 224 (2007).
6th Nanoscience and Nanotechnology Conference, zmir, 2010 808