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Molecular Imprinting

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Pressurized hot water extraction coupled to molecularly imprinted polymers for simultaneous extraction and clean-up of pesticides residues in edible and medicinal plants of the Okavango Delta, Botswana

Janes Mokgadi / Shima Batlokwa
  • Department of Earth & Environmental Science (Chemistry Unit), Botswana International University of Science & Technology, P.O. Box 041, Bontleng, Gaborone, Botswana
  • Other articles by this author:
  • De Gruyter OnlineGoogle Scholar
/ Keta Mosepele / Veronica Obuseng / Nelson Torto
Published Online: 2013-10-08 | DOI: https://doi.org/10.2478/molim-2013-0003


In this study, an in-cell extraction and clean-up approach, employing pressurized hot water extraction (PHWE) coupled to a molecularly imprinted polymer (MIP) is proposed. The selectivity of PHWE was improved through the use of a chlorophyll MIP (PHWE-MIP) for the determination of organochlorine pesticides residue levels in various edible and medicinal plants of the Okavango Delta, Botswana. The PHWE-MIP method achieved simultaneous extraction and clean-up. PHWE employed an optimal temperature of 260 °C, pressure of 90 bar and flow rate of 1 mL min-1 in 10 min for the extraction of the pesticides from plants while the MIP selectively overcame the interfering chlorophyll prior to analysis with gas chromatograph coupled to electron capture detector or mass spectrometer (GC-ECD/MS). The results obtained were compared to the QuEChERS Official Method 2007:01 for pesticides residue analysis. The proposed method seems to be nearly fully automated, environmental friendly, selective, simple and quick. Moreover, the recoveries of planar pesticides were improved (93-95%) with relative standard deviations (%RSD) of less than 10%.

Keywords: Subcritical water extraction; Molecular imprinted polymers; In-cell clean up; Sample preparation; Environmentally friendly

  • [1] A.L. Chiuchiolo, R.M. Dickhut, M.A. Cochran and H.W. Ducklow, “Persistent organic pollutants at the base of the Antarctic marine food web,” Environ. Sci. Technol, 38 (2004) 3551-3557. PubMedGoogle Scholar

  • [2] J.Weinberg, Overview of POPs and need for a POPs treaty. Public forum on persistent organic pollutants- the international POPs elimination network, 1998. Google Scholar

  • [3] P.K. Gupta, M. Hubbard, B. Gurley and H. P. Hendrickson, “Validation of a liquid chromatography-tandem mass spectrometric assay for the quantitative determination of hydrastine and berberine in human serum”, J Pharm. Biomed. Anal, 49 (2009) 1021-1026. Google Scholar

  • [4] CODEX alimentarius, (http://www.codexalimentarius.net/ mrls/pestdes/jsp/pest_q-e.jsp) Google Scholar

  • [5] X. Gong, S. Qi, Y.Wang, E.B. Julia and C. Lv, “Historical contamination and sources of organochlorine pesticides in sediment cores from Quanzhou Bay, Southeast China” Marine Pollution Bulletin, 54 (2007) 1434–1440. Web of ScienceGoogle Scholar

  • [6] C. Gonçalves, J.J. Carvalho, M.A. Azenha and M.F. Alpendurada, “Optimization of supercritical fluid extraction of pesticide residues in soil by means of central composite design and analysis by gas chromatography–tandem mass spectrometry”, J. Chromatogr. A 1110 (2006) 6-14. Google Scholar

  • [7] P. Suchan, J. Pulkrabová, J. Hajŝlová and V. Kocourek, “Pressurized liquid extraction in determination of polychlorinated biphenyls and organochlorine pesticides in fish samples”, Anal. Chim. Acta, 520 (2004) 193-200. Google Scholar

  • [8] L. Chen, L. Ding, H. Jin, D. Song, H. Zhang, J. Li, K. Zhang, Y. Wang and H. Zhang, “The determination of organochlorine pesticides based on dynamic microwave-assisted extraction coupled with on-line solid-phase extraction of highperformance liquid chromatography Anal.Chim. Acta, 589 (2007) 239-246. Google Scholar

  • [9] C. Gonçalves and M.F. Alpendurada, “Assessment of pesticide contamination in soil samples from an intensive horticulture area, using ultrasonic extraction and gas chromatography–mass spectrometry”, Talanta, 65 (2005) 1179-1189. Google Scholar

  • [10] S. Babić, M. Pertrović, M. Kaštelan-Macan, Ultrasonic solvent extraction of pesticides from soil, J. Chromatogr. A 823 (1998) 3-9. Google Scholar

  • [11] C.C. Teo, S.N. Tan, J.W.H. Yong, C.S. Hew, E.S. Ong, Pressurized hot water extraction, J. of Chromatogra. A 1217 16 (2010) 2484–2494. Google Scholar

  • [12] M. Anastassiades and S. J. Lehotay, “Fast and Easy Multiresidue Method Employment Acetonitrile Extraction/ Partitioning and “Dispersive Solid-Phase Extraction” for the Determination of Pesticide Residues in Produce”, J. AOAC Int., 86 (2003) 412- 431. Google Scholar

  • [13] A. Hubert, K.Wenzel, M. Manz, L.Weissflog,W. Engewald and G. Schüürmann, High extraction Efficiency for POPs in Real Contaminated Soil Samples Using Accelerated Solvent Extraction, Anal. Chem. 72 (2000) 1294-1300. PubMedGoogle Scholar

  • [14] Z. Sharif, Y.B.C. Man, N.S.A. Hamid, C.C. Keat, Determination of organochlorine and pyrethroid pesticides in fruit and vegetables using solid phase extraction clean-up cartridges, J. Chromatogr. A 1127 (2006) 254-261. Google Scholar

  • [15] A.B. Vega, A.G. Frenich, J.L.M. Vidal, Monitoring of pesticides in agricultural water and soil samples from Andalusia by liquid chromatography coupled to mass spectrometry, Anal. Chim. Acta 538 (2005) 117-127. Google Scholar

  • [16] M. Anastassiades, S.J. Lehotay, D. Stajnbaher, F.J. Schenck, Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solidphase extraction” for the determination of pesticide residues in produce, J AOAC Int 86 (2003) 412-431. Google Scholar

  • [17] S. J. Lehotay, K. Mastovska, A.R. Lightfield, Use of buffering and other means to improve results of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables, J. AOAC Int., 88 (2005) 615-629. Google Scholar

  • [18] M. Barriada-Pereira, M.J. González-Castro, S. Muniategui-Lorenzo, P. López-Mahía, D. Prada- Rodríguez, E. Fernández-Fernández, Determination of 21 organochlorine pesticides in tree leaves using solid-phase extraction clean-up cartridges, J. Chromatogr. A 1061 (2004) 133-139. Google Scholar

  • [19] Sellergren B (2001) In: Sellergren (ed) Molecularly imprinted polymers. Man made mimics of antibodies and their applications in analytical chemistry B, Elsevier, Amsterdam, pp 305–322 Google Scholar

  • [20] E. Concha-Gra˜na, M.I. Turnes-Carou, S. Muniategui- Lorenzo, P. López-Mahía, E. Fernández-Fernández, D. Prada-Rodríguez, Development of pressurized liquid extraction and cleanup procedures for determination of organochlorine pesticides in soils, J. Chromatogr. A 1047 (2004) 147-155. Google Scholar

  • [21] C. Baggiani, L. Anfossi L, C. Giovannoli Molecular imprinted polymers as synthetic receptors for the analysis of mycoand phyco-toxins, Analyst 133 (2008) 719–730 Web of ScienceGoogle Scholar

  • [22] B.S Batlokwa, J. Mokgadi, T. Nyokong and N. Torto, Optimal Template removal from Molecularly Imprinted Polymers by Pressurized Hot Water Extraction, Chromatographia 73 (2011) 589–593 Web of ScienceGoogle Scholar

  • [23] D. Adeyemi, J. Mokgadi, J. Darkwa. C. Anyakora, G. Ukpo, C. Turner, N. Torto, Electrospun nanofibers sorbents for pre-concentration of 1,1-dichloro-2,2 bis- (4-chlorophenyl)ethylene with subsequent desorption by pressurized hot water extraction, Chromatographia 73 (2011) 1015–1020 Web of ScienceGoogle Scholar

  • [24] B.S Batlokwa, J. Mokgadi, R. Majors, C. N. Torto, A Novel Molecularly Imprinted Polymer for the Selective Removal of Chlorophyll from Heavily Pigmented Green Plant Extracts prior to Instrumental Analysis, Hindawi Publishing Corporation, Journal of Chemistry, Volume 2013, Article ID 540240, 4 pages,http://dx.doi. org/10.1155/2013/540240 Web of ScienceGoogle Scholar

  • [25] L.Mmualefe, Sample preparation for pesticide analysis in water and sediments: A case study of the Okavango Delta, Botswana, Doctoral Thesis, Rhodes University, 2010. Google Scholar

  • [26] L.C. Mmualefe N. Torto, P. Huntsman-Mapila, B. Mbongwe, Headspace solid phase microextraction in the determination of pesticides in water samples from the Okavango Delta with gas chromatography-electron capture detection and time-offlight mass spectrometry Microchemical Journal 91(2009) 239-244. Google Scholar

  • [27] P.S. Daka, V.C. Obuseng, N. Torto, P. Huntsman-Mapila, Deltamethrin in sediment samples of the Okavango Delta, Botswana, Water SA 32 (2006) 483-488. Google Scholar

  • [28] M.L.H. Mabaso, B. Sharp, C. Lengeler, Historical review of malarial control in southern African with emphasis on the use of indoor residual house-spraying, Trop. Med. Int. Health 9 (2004) 846-856. PubMedGoogle Scholar

  • [29] http://www.dionex.com/en-us/webdocs/68591-EPA-3545- ASE.pdf. Google Scholar

About the article

Received: 2013-03-15

Accepted: 2013-08-28

Published Online: 2013-10-08

Citation Information: Molecular Imprinting, Volume 1, Pages 55–64, ISSN (Online) 2084-8803, DOI: https://doi.org/10.2478/molim-2013-0003.

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©2014 Janes Mokgadi et al.. This article is distributed under the terms of the Creative Commons Attribution Non-Commercial No-Derivatives License, which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited. BY-NC-ND 3.0

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