Abstract
Magnetic polymer nanospheres were prepared and used as adsorbents for the extraction of organochlorine and pyrethroid pesticides from water samples. The adsorbents were synthesized by miniemulsion polymerization of N-vinylimidazole and divinylbenzene and simultaneous encapsulation of oleic acid-coated Fe3O4 nanoparticles. Following desorption with ethyl acetate, the target analytes β-hexachlorocyclohexane, δ-hexachlorocyclohexane, p,p’-DDE, heptachlor, trans-chlordan, cis-chlordan, bifenthrin, β-cypermethrin, δ-methrin, λ-cyhalothrin and esfenvalerate were determined by gas chromatography with electron capture detection. Desorption conditions, extraction times and sample volume were screened by Plackett-Burman design and optimized by Box-Behnken design. Under the optimum conditions, the organochlorines can be quantified in the 20 to 400 ng L−1 concentration range, and the pyrethroids in the 400 to 4000 ng L−1 concentration range. The recoveries of organochlorines and pyrethroids from spiked real water samples are between 77.6 and 97.3 %, with relative standard deviations between 0.9 and 10.0 %. The method for magnetic solid phase extraction described here is fast, simple and friendly to the environment.
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References
Borga K, Gabrielsen GW, Skaare JU (2001) Biomagnification of organochlorines along a Barents Sea food chain. Environ Pollut 113(2):187–198
Longanathan BG, Kannan K (1994) Global oganochlorine contamination trends: an overview. Ambio 23(3):187–191
Zhou R, Zhu L, Yang K, Chen Y (2006) Distribution of organochlorine pesticides in surface water and sediments from Qiantang River, East China. J Hazard Mater 137(1):68–75
X-h L, Wang W, Wang J, Cao X-l, Wang X-f, Liu J-c, Liu X-f, Xu X-b, Jiang X-n (2008) Contamination of soils with organochlorine pesticides in urban parks in Beijing, China. Chemosphere 70(9):1660–1668
Berzas Nevado JJ, Rodriguez Martin-Doimeadios RC, Guzman Bernardo FJ, Rodriguez Farinas N, Gonzalez Cogolludo JM, Castro Osma JA (2010) Multiresidue determination of organochlorines in fish oil by GC MS: a new strategy in the sample preparation. Talanta 81(3):887–893
Li J, Liu D, Wu T, Zhao W, Zhou Z, Wang P (2014) A simplified procedure for the determination of organochlorine pesticides and polychlorobiphenyls in edible vegetable oils. Food Chem 151:47–52
Yu Y, Li Y, Shen Z, Yang Z, Mo L, Kong Y, Lou I (2014) Occurrence and possible sources of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) along the Chao River, China. Chemosphere 114:136–143
Grung M, Lin Y, Zhang H, Steen AO, Huang J, Zhang G, Larssen T (2015) Pesticide levels and environmental risk in aquatic environments in China - A review. Environ Int 81:87–97
Yadav IC, Devi NL, Syed JH, Cheng Z, Li J, Zhang G, Jones KC (2015) Current status of persistent organic pesticides residues in air, water, and soil, and their possible effect on neighboring countries: a comprehensive review of India. Sci Total Environ 511:123–137
Zhang H, Bayen S, Kelly BC (2015) Multi-residue analysis of legacy POPs and emerging organic contaminants in Singapore’s coastal waters using gas chromatography-triple quadrupole tandem mass spectrometry. Sci Total Environ 523:219–232
Derbalah A, Ismail A, Hamza A, Shaheen S (2014) Monitoring and remediation of organochlorine residues in water. Water Environ Res 86(7):584–593
Isman MB (2006) Botanical insecticides, deterrents, and repellents in modern agriculture and an increasingly regulated world. Ann Rev of Entomol: 45–66
Feo ML, Eljarrat E, Barcelo D (2010) A rapid and sensitive analytical method for the determination of 14 pyrethroids in water samples. J Chromatogr A 1217(15):2248–2253
Feo ML, Ginebreda A, Eljarrat E, Barcelo D (2010) Presence of pyrethroid pesticides in water and sediments of Ebro River Delta. J Hydrol 393(3–4):156–162
Hladik ML, Kuivila KM (2009) Assessing the occurrence and distribution of pyrethroids in water and suspended sediments. J Agric Food Chem 57(19):9079–9085
Richter BE, Jones BA, Ezzell JL, Porter NL, Avdalovic N, Pohl C (1996) Accelerated solvent extraction: a technique for sample preparation. Anal Chem 68(6):1033–1039
Herrera-Herrera AV, Asensio-Ramos M, Hernandez-Borges J, Rodriguez-Delgado MA (2010) Dispersive liquid-liquid microextraction for determination of organic analytes. Trac-Trends Anal Chem 29(7):728–751
Beltran J, Lopez FJ, Hernandez F (2000) Solid-phase microextraction in pesticide residue analysis. J Chromatogr A 885(1–2):389–404
Capriotti AL, Cavaliere C, Lagana A, Piovesana S, Samperi R (2013) Recent trends in matrix solid-phase dispersion. Trac-Trends Anal Chem 43:53–66
Safarikova M, Safarik I (1999) Magnetic solid-phase extraction. J Magn Magn Mater 194(1–3):108–112
He Z, Wang P, Liu D, Zhou Z (2014) Hydrophilic-lipophilic balanced magnetic nanoparticles: preparation and application in magnetic solid-phase extraction of organochlorine pesticides and triazine herbicides in environmental water samples. Talanta 127:1–8
Gao Q, Zheng H-B, Luo D, Ding J, Feng Y-Q (2012) Facile synthesis of magnetic one-dimensional polyaniline and its application in magnetic solid phase extraction for fluoroquinolones in honey samples. Anal Chim Acta 720:57–62
Yu X, Sun Y, Jiang C, Sun X, Gao Y, Wang Y, Zhang H, Song D (2012) Magnetic solid-phase extraction of five pyrethroids from environmental water samples followed by ultrafast liquid chromatography analysis. Talanta 98:257–264
Aziz-Zanjani MO, Mehdinia A (2014) A review on procedures for the preparation of coatings for solid phase microextraction. Microchim Acta 181(11–12):1169–1190
Huang X, Wang Y, Liu Y, Yuan D (2013) Preparation of magnetic poly(vinylimidazole-co-divinylbenzene) nanoparticles and their application in the trace analysis of fluoroquinolones in environmental water samples. J Sep Sci 36(19):3210–3219
Yan S, Gao Z, Fang Y, Cheng Y, Zhou H, Wang H (2007) Characterization and quality assessment of binding properties of malachite green molecularly imprinted polymers prepared by precipitation polymerization in acetonitrile. Dyes Pigments 74:572–577
Huang B, Zhou X, Chen J, Wu G, Lu X (2015) Determination of malachite green in fish based on magnetic molecularly imprinted polymer extraction followed by electrochemiluminescence. Talanta 142:228–234
Wang C, Hu X, Guan P, Qian L, Wu D, Li J (2015) Superparamagnetic molecularly imprinting polymers for adsorbent and separation pentapeptides by surface ATRP. Sep Sci Technol 50(12):1768–1775
Zuo HG, Zhu JX, Zhan CR, Shi L, Xing M, Guo P, Ding Y, Yang H (2015) Preparation of malathion MIP-SPE and its application in environmental analysis. Environ Monit Assess 187(7)
Lin S, Gan N, Zhang J, Chen X, Cao Y, Li T (2015) A novel reductive graphene oxide-based magnetic molecularly imprinted poly (ethylene-co-vinyl alcohol) polymers for the enrichment and determination of polychlorinated biphenyls in fish samples. J Mol Recog 28(6):359–368
Chen F, Zhang J, Wang M, Kong J (2015) Magnetic molecularly imprinted polymers synthesized by surface-initiated reversible addition-fragmentation chain transfer polymerization for the enrichment and determination of synthetic estrogens in aqueous solution. J Sep Sci 38(15):2670–2676
Shao Y, Zhou L, Bao C, Ma J (2015) A facile approach to the fabrication of rattle-type magnetic carbon nanospheres for removal of methylene blue in water. Carbon 89:378–391
Pérez RA, Albero B, Tadeo JL, Sánchez-Brunete C (2015) Oleate functionalized magnetic nanoparticles as sorbent for the analysis of polychlorinated biphenyls in juices. Microchimica Acta
Safari M, Yamini Y, Tahmasebi E, Ebrahimpour B (2015) Magnetic nanoparticle assisted supramolecular solvent extraction of triazine herbicides prior to their determination by HPLC with UV detection. Microchimica Acta
Shulai L, Forcada J (2006) Preparation and characterization of magnetic polymeric composite particles by miniemulsion polymerization. J Polym Sci A Polym Chem 44(13):4187–4203
Li C, Chen L (2013) Determination of pyrethroid pesticides in environmental waters based on magnetic titanium dioxide nanoparticles extraction followed by HPLC analysis. Chromatographia 76(7–8):409–417
Fang G, Chen W, Yao Y, Wang J, Qin J, Wang S (2012) Multi-residue determination of organophosphorus and organochlorine pesticides in environmental samples using solid-phase extraction with cigarette filter followed by gas chromatography–mass spectrometry. J Sep Sci 35(4):534–540
Ozcan S, Tor A, Aydin ME (2012) Application of magnetic nanoparticles to residue analysis of organochlorine pesticides in water samples by GC/MS. J Aoac Int 95(5):1343–1349(1347)
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Supported by the National Natural Science Foundation of China (J1210064,21277171,21307155), Chinese Universities Scientific Fund 2015LX005 and Beijing Nova program YETP0323.
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Yang, G., He, Z., Liu, X. et al. Polymer-coated magnetic nanospheres for preconcentration of organochlorine and pyrethroid pesticides prior to their determination by gas chromatography with electron capture detection. Microchim Acta 183, 1187–1194 (2016). https://doi.org/10.1007/s00604-015-1725-z
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DOI: https://doi.org/10.1007/s00604-015-1725-z