Abstract
In this research, a novel nanocomposite based on incorporation of graphene oxide (GO) into polyamide (PA) was prepared by solvent blending method and subsequently it was coated on stir bar substrate through solvent exchange method. The morphology and surface characteristic of PA- and GO/PA-coated stir bars were investigated using scanning electron microscopy (SEM). The prepared GO/PA nanocomposite-based stir bar was applied as an extraction device for stir bar sorptive extraction (SBSE) of organophosphorous pesticides (OPPs) including chlorpyrifos, ethion, and phosalone in fruit juice and vegetable samples followed by gas chromatography–flame ionization detector (GC-FID) detection. The effect of GO doping level into the nanocomposite on the extraction capability of the coating was investigated. Important factors influencing the extraction and desorption processes including extraction time, salt content, sample volume, pH, desorption solvent, its volume, and desorption time were studied and optimized applying central composite design (CCD). Limits of detection (LOD) and linear dynamic ranges of the method were in the range of 0.3–1 ng mL−1 and 1–1000 and 3–1000 ng mL−1, respectively. The method precision (RSD%) with four replicate determinations was in the range of 6.2–9.1% for distilled water at the concentration level of 100 ng mL−1. The developed method was successfully applied to various fruit juices and vegetable samples, while the relative recoveries (RR %) were found to be in the range of 82.0–95.6%.
Graphical abstract
Similar content being viewed by others
References
Bagheri H, Ayazi Z, Es-haghi A, Aghakhani A (2012) Reinforced polydiphenylamine nanocomposite for microextraction in packed syringe of various pesticides. J Chromatogr A 1222:13–21
Bagheri H, Ayazi Z, Aghakhani A (2011) A novel needle trap sorbent based on carbon nanotube-sol-gel for microextraction of polycyclic aromatic hydrocarbons from aquatic media. Anal Chim Acta 683(2):212–220
Zhu Y, Murali S, Cai W, Li X, Suk JW, Potts JR, Ruoff RS (2010) Graphene and graphene oxide: synthesis, properties, and applications. Adv Mater 22(35):3906–3924
Su Q, Pang S, Alijani V, Li C, Feng X, Mullen K (2009) Composites of graphene with large aromatic molecules. Adv Mater 21(31):3191–3195
Loh KP, Bao Q, Ang PK, Yang J (2010) The chemistry of graphene. J Mater Chem 20(12):2277–2289
Zacharia R, Ulbricht H, Hertel T (2004) Interlayer cohesive energy of graphite from thermal desorption of polyaromatic hydrocarbons. Phys Rev B 69(15):155406
Baltussen E, Sandra P, David F, Cramers C (1999) Stir bar sorptive extraction (SBSE), a novel extraction technique for aqueous samples: theory and principles. J Microcolumn Sep 11(10):737–747
Guerrero EDN, Maran RN, Mejuas RC, Barroso CG (2007) Stir bar sorptive extraction of volatile compounds in vinegar: validation study and comparison with solid phase microextraction. J Chromatogr A 1167(1):18–26
He M, Chen B, Hu B (2014) Recent developments in stir bar sorptive extraction. Anal Bioanal Chem 406(8):2001–2026
Fontanals N, Marce RM, Borrull F (2007) New materials in sorptive extraction techniques for polar compounds. J Chromatogr A 1152(1):14–31
Huang X, Qiu N, Yuan D, Lin Q (2009) Sensitive determination of strongly polar aromatic amines in water samples by stir bar sorptive extraction based on poly (vinylimidazole-divinylbenzene) monolithic material and liquid chromatographic analysis. J Chromatogr A 1216(20):4354–4360
Neng NR, Pinto ML, Pires J, Marcos PM, Nogueira JMF (2007) Development, optimisation and application of polyurethane foams as new polymeric phases for stir bar sorptive extraction. J Chromatogr A 1171(1):8–14
Silva ARM, FtCM Portugal, Nogueira JMF (2008) Advances in stir bar sorptive extraction for the determination of acidic pharmaceuticals in environmental water matrices: comparison between polyurethane and polydimethylsiloxane polymeric phases. J Chromatogr A 1209(1):10–16
Liu W, Wang H (1045) Guan Y (2004) Preparation of stir bars for sorptive extraction using sol-gel technology. J Chromatogr A 1:15–22
Ayazi Z, Rafighi P (2015) Preparation and application of a carbon nanotube reinforced polyamide-based stir bar for sorptive extraction of naproxen from biological samples prior to its spectrofluorometric determination. Anal Methods 7(7):3200–3210
Bagheri H, Ayazi Z, Babanezhad E (2010) A sol-gel-based amino functionalized fiber for immersed solid-phase microextraction of organophosphorus pesticides from environmental samples. Microchem J 94(1):1–6
Bagheri H, Aghakhani A, Akbari M, Ayazi Z (2011) Electrospun composite of polypyrrole-polyamide as a micro-solid phase extraction sorbent. Anal Bioanal Chem 400(10):3607–3613
Bagheri H, Ayazi Z, Aghakhani A, Alipour N (2012) Polypyrrole/polyamide electrospun-based sorbent for microextraction in packed syringe of organophosphorous pesticides from aquatic samples. J Sep Sci 35(1):114–120
Bagheri H, Aghakhani A, Ayazi Z, Khakinezhad M (2011) A polypyrrole-based sorptive microextraction coating for preconcentration of malathion from aquatic media. Chromatographia 74(9–10):731–735
Hummers WS Jr, Offeman RE (1958) Preparation of graphitic oxide. J Am Chem Soc 80(6):1339
Ayazi Z, Khoshhesab ZM, Norouzi S (2016) Modeling and optimizing of adsorption removal of Reactive Blue 19 on the magnetite/graphene oxide nanocomposite via response surface methodology. Desalination Water Treat:1-16
Ayazi Z, Matin AA (2016) Development of carbon nanotube-polyamide nanocomposite-based stir bar sorptive extraction coupled to HPLC-UV applying response surface methodology for the analysis of bisphenol A in aqueous samples. J Chromatogr Sci 54:1841–1850
Quintana JB, Rodil R, Muniategui-Lorenzo S, Pn Lupez-Mahua, Prada-Rodroguez D (2007) Multiresidue analysis of acidic and polar organic contaminants in water samples by stir-bar sorptive extraction-liquid desorption-gas chromatography-mass spectrometry. J Chromatogr A 1174(1):27–39
Ochiai N, Sasamoto K, Kanda H, Nakamura S (2006) Fast screening of pesticide multiresidues in aqueous samples by dual stir bar sorptive extraction-thermal desorption-low thermal mass gas chromatography-mass spectrometry. J Chromatogr A 1130(1):83–90
Bagheri H, Ayazi Z, Sistani H (2011) Chemically bonded carbon nanotubes on modified gold substrate as novel unbreakable solid phase microextraction fiber. Microchim Acta 174(3–4):295–301
Zuin VG, Montero L, Bauer C, Popp P (2005) Stir bar sorptive extraction and high-performance liquid chromatography-fluorescence detection for the determination of polycyclic aromatic hydrocarbons in Mate teas. J Chromatogr A 1091(1):2–10
Bagheri H, Sistani H, Ayazi Z (2011) Novel unbreakable solid-phase microextraction fiber by electrodeposition of silica sol-gel on gold. J Sep Sci 34(22):3246–3252
Blasco C, Fernandez M, Pico Y, Font G (2004) Comparison of solid-phase microextraction and stir bar sorptive extraction for determining six organophosphorus insecticides in honey by liquid chromatography-mass spectrometry. J Chromatogr A 1030(1):77–85
León VM, Alvarez B, Cobollo MA, Munoz S, Valor I (2003) Analysis of 35 priority semivolatile compounds in water by stir bar sorptive extraction–thermal desorption–gas chromatography–mass spectrometry: I. Method optimisation. J Chromatogr A 999(1):91–101
Okubo M, Ichikawa K, Tsujihiro M, He Y (1990) Production of anomalous polymer microspheres having uneven surfaces by stepwise heterocoagulation technique. Colloid Polym Sci 268(9):791–796
Zambonin CG, Quinto M, De Vietro N, Palmisano F (2004) Solid-phase microextraction-gas chromatography mass spectrometry: a fast and simple screening method for the assessment of organophosphorus pesticides residues in wine and fruit juices. Food Chem 86(2):269–274
Bai Y, Zhou L, Wang J (2006) Organophosphorus pesticide residues in market foods in Shaanxi area, China. Food Chem 98(2):240–242
Liu M, Yuki H, Song Y, Lin J (2006) Determination of carbamate and organophosphorus pesticides in fruits and vegetables using liquid chromatography-mass spectrometry with dispersive solid phase extraction. Chin J Anal Chem 34(7):941–945
Kumari B, Madan VK, Singh J, Singh S, Kathpal TS (2004) Monitoring of pesticidal contamination of farmgate vegetables from Hisar. Environ Monit Assess 90(1–3):65–71
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of interest
Zahra Ayazi declares that she has no conflict of interest. Raana Jafarzadeh declares that she has no conflict of interest.
Ethical approval
This article does not contain any studies with human participants or animals performed by any of the authors.
Funding
The financial support of this work was provided by the Research Council of Azarbaijan Shahid Madani University.
Informed consent
Not applicable.
Rights and permissions
About this article
Cite this article
Ayazi, Z., Jaafarzadeh, R. Graphene Oxide/Polyamide Nanocomposite as a Novel Stir Bar Coating for Sorptive Extraction of Organophosphorous Pesticides in Fruit Juice and Vegetable Samples. Chromatographia 80, 1411–1422 (2017). https://doi.org/10.1007/s10337-017-3364-5
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10337-017-3364-5