Abstract
A selective and sensitive magnetic dispersive solid-phase microextraction (MDSPME) coupled with gas chromatography-mass spectrometry was developed for extraction and determination of organophosphorus pesticides (Sevin, Fenitrothion, Malathion, Parathion, and Diazinon) in fruit juice and real water samples. Zero valent Fe-reduced graphene oxide quantum dots (rGOQDs@ Fe) as a new and effective sorbent were prepared and applied for extraction of organophosphorus pesticides using MDSPME method. In order to study the performance of this new sorbent, the ability of rGOQDs@ Fe was compared with graphene oxide and magnetic graphene oxide nanocomposite by recovery experiments of the organophosphorus pesticides. Several affecting parameters in the microextraction procedure, including pH of donor phase, donor phase volume, stirring rate, extraction time, and desorption conditions such as the type and volume of solvents and desorption time were thoroughly investigated and optimized. Under the optimal conditions, the method showed a wide linear dynamic range with R-square between 0.9959 and 0.9991. The limit of detections, the intraday and interday relative standard deviations (n = 5) were less than 0.07 ngmL–1, 4.7, and 8.6%, respectively. The method was successfully applied for extraction and determination of organophosphorus pesticides in real water samples (well, river and tap water) and fruit juice samples (apple and grape juice). The obtained relative recoveries were in the range of 82.9%–113.2% with RSD percentages of less than 5.8% for all the real samples.
Similar content being viewed by others
References
Yang Y, Asiri AM, Du D, Lin Y. Acetylcholinesterase biosensor based on a gold nanoparticle–polypyrrole–reduced graphene oxide nanocomposite modified electrode for the amperometric detection of organophosphorus pesticides. Analyst. 2014;139(12):3055–60.
Berijani S, Sadigh M, Pournamdari E. Homogeneous liquid–liquid microextraction for determination of organophosphorus pesticides in environmental water samples prior to gas chromatography-flame photometric detection. J Chromatogr Sci. 2016;54:1061–7.
Fulco CE, Liverman CT, Sox HC, Effects of long-term exposure to organophosphate pesticides in humans.National Academies Press (US); 2000.
Deng X, Guo Q, Chen X, Xue T, Wang H, Yao P. Rapid and effective sample clean-up based on magnetic multiwalled carbon nanotubes for the determination of pesticide residues in tea by gas chromatography–mass spectrometry. Food Chem. 2014;145:853–8.
Zhang W, Asiri AM, Liu D, Du D, Lin Y. Nanomaterial-based biosensors for environmental and biological monitoring of organophosphorus pesticides and nerve agents. Trends Anal Chem. 2014;54:1–10.
Meng X, Wei J, Ren X, Ren J, Tang F. A simple and sensitive fluorescence biosensor for detection of organophosphorus pesticides using H 2 O 2-sensitive quantum dots/bi-enzyme. Biosens Bioelectron. 2013;47:402–7.
Ghorbani M, Chamsaz M, Rounaghi GH. Glycine functionalized multiwall carbon nanotubes as a novel hollow fiber solid-phase microextraction sorbent for pre-concentration of venlafaxine and o-desmethylvenlafaxine in biological and water samples prior to determination by high-performance liquid chromatography. Anal Bioanal Chem. 2016;408(16):4247–56.
Ghorbani M, Chamsaz M, Rounaghi GH. Ultrasound-assisted magnetic dispersive solid-phase microextraction: a novel approach for the rapid and efficient microextraction of naproxen and ibuprofen employing experimental design with high-performance liquid chromatography. J Sep Sci. 2016;39(6):1082–9.
Mahpishanian S, Sereshti H. Graphene oxide-based dispersive micro-solid phase extraction for separation and preconcentration of nicotine from biological and environmental water samples followed by gas chromatography-flame ionization detection. Talanta. 2014;130:71–7.
Wen Y, Niu Z, Ma Y, Ma J, Chen L. Graphene oxide-based microspheres for the dispersive solid-phase extraction of nonsteroidal estrogens from water samples. J Chromatogr A. 2014;1368:18–25.
Chen D, Zhao Y, Miao H, Wu Y. A novel dispersive micro solid phase extraction using PCX as the sorbent for the determination of melamine and cyromazine in milk and milk powder by UHPLC-HRMS/MS. Talanta. 2015;134:144–52.
Zhu F, Ruan W, He M, Zeng F, Luan T, Tong Y, et al. Application of solid-phase microextraction for the determination of organophosphorus pesticides in textiles by gas chromatography with mass spectrometry. Anal Chim Acta. 2009;650(2):202–6.
Xie J, Liu T, Song G, Hu Y, Deng C. Simultaneous analysis of organophosphorus pesticides in water by magnetic solid-phase extraction coupled with GC-MS. Chromatographia. 2013;76(9/10):535–40.
Fenik J, Tankiewicz M, Biziuk M. Properties and determination of pesticides in fruits and vegetables. Trends Anal Chem. 2011;30(6):814–26.
Mehdinia A, Aziz-Zanjani MO. Recent advances in nanomaterials utilized in fiber coatings for solid-phase microextraction. Trends Anal Chem. 2013;42:205–15.
Tian J, Xu J, Zhu F, Lu T, Su C, Ouyang G. Application of nanomaterials in sample preparation. J Chromatogr A. 2013;1300:2–16.
Esmaeili A, Entezari MH. Facile and fast synthesis of graphene oxide nanosheets via bath ultrasonic irradiation. J Colloid Interface Sci. 2014;432:19–25.
Liu Y, Deng R, Wang Z, Liu H. Carboxyl-functionalized graphene oxide–polyaniline composite as a promising supercapacitor material. J Mater Chem. 2012;22(27):13619–24.
Karamani AA, Douvalis AP, Stalikas CD. Zero-valent iron/iron oxide-oxyhydroxide/graphene as a magnetic sorbent for the enrichment of polychlorinated biphenyls, polyaromatic hydrocarbons and phthalates prior to gas chromatography-mass spectrometry. J Chromatogr A. 2013;1271(1):1–9.
Shi Y, Pramanik A, Tchounwou C, Pedraza F, Crouch RA, Chavva SR, et al. Multifunctional biocompatible graphene oxide quantum dots decorated magnetic nanoplatform for efficient capture and two-photon imaging of rare tumor cells. ACS Appl Mater Interfaces. 2015;7(20):10935–43.
Pawliszyn J, Handbook of solid phase microextraction. 1ed. Elsevier; 2012.
Wercinski SA , Solid phase microextraction: a practical guide. CRC Press:Taylor & Francis Group; 1999.
Es’haghi Z, Khalili M, Khazaeifar A, Rounaghi GH. Simultaneous extraction and determination of lead, cadmium, and copper in rice samples by a new preconcentration technique: hollow fiber solid phase microextraction combined with differential pulse anodic stripping voltammetry. Electrochim Acta. 2011;56(9):3139–46.
Song X-Y, Shi Y-P, Chen J. A novel extraction technique based on carbon nanotubes reinforced hollow fiber solid/liquid microextraction for the measurement of piroxicam and diclofenac combined with high performance liquid chromatography. Talanta. 2012;100:153–61.
Sun J, Liang Q, Han Q, Zhang X, Ding M. One-step synthesis of magnetic graphene oxide nanocomposite and its application in magnetic solid phase extraction of heavy metal ions from biological samples. Talanta. 2015;132:557–63.
Wang C, Feng C, Gao Y, Ma X, Wu Q, Wang Z. Preparation of a graphene-based magnetic nanocomposite for the removal of an organic dye from aqueous solution. Chem Eng J. 2011;173(1):92–7.
Armbruster DA, Pry T. Limit of blank, limit of detection, and limit of quantitation. Clin Biochem Rev. 2008;29(Suppl 1):S49–52.
Fadaei A, Dehghani MH, Nasseri S, Mahvi AH, Rastkari N, Shayeghi M. Organophosphorous pesticides in surface water of Iran. Bull Environ Contam Toxicol. 2012;88(6):867–9.
Ballesteros E, Parrado M. Continuous solid-phase extraction and gas chromatographic determination of organophosphorus pesticides in natural and drinking waters. J Chromatogr A. 2004;1029(1):267–73.
Ravelo-Pérez LM, Hernández-Borges J, Ángel Rodríguez-Delgado M. Multiwalled carbon nanotubes as solid-phase extraction materials for the gas chromatographic determination of organophosphorus pesticides in waters. J Sep Sci. 2008;31(20):3612–9.
Su R, Xu X, Wang X, Li D, Li X, Zhang H, et al. Determination of organophosphorus pesticides in peanut oil by dispersive solid phase extraction gas chromatography-mass spectrometry. J Chromatogr B. 2011;879(30):3423–8.
You X, Xing Z, Liu F, Jiang N. Air-assisted liquid–liquid microextraction used for the rapid determination of organophosphorus pesticides in juice samples. J Chromatogr A. 2013;1311:41–7.
Wang Q, Yin J, Pan H, Xu F, Yang Y. A novel method based on combining ultrasonic-assisted dispersive solid-phase extraction and low-density solvent dispersive liquid–liquid microextraction (UA-DSPE-LDS-DLLME) for the determination of organophosphorus pesticides in soil. Anal Methods. 2014;6(18):7335–42.
Acknowledgements
The authors gratefully acknowledge the support of this research by the Ferdowsi University of Mashhad, Mashhad, Iran (No. 3/32788 dated 12/04/2014) and Central Lab Rural Water and Waste Water Company, Khorasan Razavi, Iran.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
This article does not contain any studies with animal or human subjects.
Conflict of interest
The authors declare no conflict of interest.
Electronic supplementary material
ESM 1
(PDF 153 KB)
Rights and permissions
About this article
Cite this article
Akbarzade, S., Chamsaz, M., Rounaghi, G.H. et al. Zero valent Fe-reduced graphene oxide quantum dots as a novel magnetic dispersive solid phase microextraction sorbent for extraction of organophosphorus pesticides in real water and fruit juice samples prior to analysis by gas chromatography-mass spectrometry. Anal Bioanal Chem 410, 429–439 (2018). https://doi.org/10.1007/s00216-017-0732-9
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00216-017-0732-9