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In-needle Microextraction Coupled with Gas Chromatography/Mass Spectrometry for the Analysis of Phthalates Generating from Food Containers

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Abstract

In this study, we fabricated a new device for headspace in-needle microextraction using a stainless steel wire coated with multiwalled carbon nanotube/polyaniline composite by coulometric technique. Then, the coated wire was placed into a stainless steel needle inside. This headspace in-needle microextraction device was applied for the determination of phthalates dissolved in aqueous solution by gas chromatography-mass spectrometry. Multiwalled carbon nanotube/polyaniline composite film of 10 mm length on the surface of stainless steel wire was optimized to polymerize electrochemically when constant potential of 2.0 V was applied during 500 s. Atomic force microscopy and Auger electron spectroscopy showed that polymerization on the surface of wire had smooth, homogeneous, and constant coating thickness of 1.5 ± 0.004 μm. The optimum molar ratio of multiwalled carbon nanotube and aniline (C:N) for polymerization was determined at 1: 2 M ratio. The optimum conditions of the proposed method were extraction temperature 50 °C, saturation time 60 min, extraction time 30 min, desorption temperature 230 °C, and desorption time 3 min, respectively. Validation of headspace in-needle microextraction-multiwalled carbon nanotube/polyaniline coupled with GC/MS was also performed including limit of detection, limit of quantitation, dynamic range, recovery, and reproducibility. The proposed device is found to be inexpensive, easy, and rapid to fabricate and could be utilized effectively as the solventless microextraction method for the analysis of phthalates generating from food containers.

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References

  • Ai Y, Wu M, Li L, Zhao F, Zeng B (2016) Highly selective and effective solid phase microextraction of benzoic acid esters using ionic liquid functionalized multiwalled carbon nanotubes-doped polyaniline coating. J Chromatogr A 1437:1–7

    Article  CAS  PubMed  Google Scholar 

  • Asadollahzadeh H, Noroozian E, Maghsoudi S (2010) Solid-phase microextraction of phthalate esters from aqueous media by electrochemically deposited carbon nanotube/polypyrrole composite on a stainless steel fiber. Anal Chim Acta 669:32–38

    Article  CAS  PubMed  Google Scholar 

  • Autian J (1973) Toxicity and health threats of phthalate esters: review of the literature. Environ Health Perspect 4:3–26

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  • Bang Y, Hwang Y, Lee S, Park S, Bae S (2017) Sol-gel adsorbent-coated extraction needles to detect volatile compounds in spoiled fish. J Sep Sci 40:3839–3847

    Article  CAS  PubMed  Google Scholar 

  • Cai Y, Jiang G, Liu J, Zhou Q (2003) Multiwalled carbon nanotubes as a solid-phase extraction adsorbent for the determination of bisphenol A, 4-n-nonylphenol, and 4-tert-octylphenol. Anal Chem 75:2517–2521

    Article  CAS  PubMed  Google Scholar 

  • Cao X (2008) Determination of phthalates and adipate in bottled water by headspace solid-phase microextraction and gas chromatography/mass spectrometry. J Chromatogr A 1178:231–238

    Article  CAS  PubMed  Google Scholar 

  • Carnol L, Schummer C, Moris G (2017) Quantification of six phthalates and one adipate in Luxembourgish beer using HS-SPME-GC/MS. Food Anal Methods 10:298–309

    Article  Google Scholar 

  • Castillo M, Oubina A, Barceló D (1998) Evaluation of ELISA kits followed by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry for the determination of organic pollutants in industrial effluents. Environ Sci Technol 32:2180–2184

    Article  CAS  Google Scholar 

  • Chen GZ, Shaffer MS, Coleby D, Dixon G, Zhou W, Fray DJ, Windle AH (2000) Carbon nanotube and polypyrrole composites: coating and doping. Adv Mater 12:522–526

    Article  CAS  Google Scholar 

  • Colon I, Dimandja JD (2004) High-throughput analysis of phthalate esters in human serum by direct immersion SPME followed by isotope dilution–fast GC/MS. Anal Bioanal Chem 380:275–283

    Article  CAS  PubMed  Google Scholar 

  • Dhand C, Arya SK, Singh SP, Singh BP, Datta M, Malhotra B (2008) Preparation of polyaniline/multiwalled carbon nanotube composite by novel electrophoretic route. Carbon 46:1727–1735

    Article  CAS  Google Scholar 

  • Ding R, Lu G, Yan Z, Wilson MJ (2001) Recent advances in the preparation and utilization of carbon nanotubes for hydrogen storage. Nanosci Nanotechnol 1:7–29

    Article  CAS  Google Scholar 

  • Du W, Zhao F, Zeng B (2009) Novel multiwalled carbon nanotubes–polyaniline composite film coated platinum wire for headspace solid-phase microextraction and gas chromatographic determination of phenolic compounds. J Chromatogr A 1216:3751–3757

    Article  CAS  PubMed  Google Scholar 

  • Fan J, Wan M, Zhu D, Chang B, Pan Z, Xie S (1999) Synthesis and properties of carbon nanotube-polypyrrole composites. Synth Met 102:1266–1267

    Article  CAS  Google Scholar 

  • Feng Y, Zhu J, Sensenstein R (2005) Development of a headspace solid-phase microextraction method combined with gas chromatography mass spectrometry for the determination of phthalate esters in cow milk. Anal Chim Acta 538:41–48

    Article  CAS  Google Scholar 

  • Fernández-Amado M, Prieto-Blanco M, López-Mahía P, Muniategui-Lorenzo S, Prada-Rodríguez D (2016) Strengths and weaknesses of in-tube solid-phase microextraction: a scoping review. Anal Chim Acta 906:41–57

    Article  CAS  PubMed  Google Scholar 

  • Gharari H, Farjaminezhad M, Marefat A, Fakhari AR (2016) All-in-one solid-phase microextraction: development of a selective solid-phase microextraction fiber assembly for the simultaneous and efficient extraction of analytes with different polarities. J Sep Sci 39:1709–1716

    Article  CAS  PubMed  Google Scholar 

  • Hüffer T, Osorio XL, Jochmann MA, Schilling B, Schmidt TC (2013) Multi-walled carbon nanotubes as sorptive material for solventless in-tube microextraction (ITEX2)—a factorial design study. Anal Bioanal Chem 405:8387–8395

    Article  CAS  PubMed  Google Scholar 

  • Hwang YR, Bae S (2017) Needle fabrication method of polymeric adsorbent coated inside and its micro-extraction method. Korean patent 10-2016-0074965

  • Jeon HR, Son HH, Bae S, Lee DS (2015) Use of polyacrylic acid and polydimethylsiloxane mixture for in-needle microextraction of volatile aroma compounds in essential oils. Bull Kor Chem Soc 36:2730–2739

    Article  CAS  Google Scholar 

  • Jobling S, Reynolds T, White R, Parker MG, Sumpter JP (1995) A variety of environmentally persistent chemicals, including some phthalate plasticizers, are weakly estrogenic. Environ Health Perspect 103:582–587

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  • Kamrin MA (2009) Phthalate risks, phthalate regulation, and public health: a review. J Toxicol Environ Health B 12:157–174

    Article  CAS  Google Scholar 

  • Lee EJ, Lee DS (2014) Fabrication of in-needle microextraction device using nichrome wire coated with poly(ethylene glycol) and poly(dimethylsiloxane) for determination of volatile compounds in lavender oils. Bull Kor Chem Soc 35:211–217

    Article  CAS  Google Scholar 

  • Louch D, Motlagh S, Pawliszyn J (1992) Dynamics of organic compound extraction from water using liquid-coated fused silica fibers. Anal Chem 64:1187–1199

    Article  CAS  Google Scholar 

  • McNaught AD, Wilkinson A (1997) Compendium of chemical terminology. IUPAC recommendations

  • Moliner-Martinez Y, Herráez-Hernández R, Verdú-Andrés J, Molins-Legua C, Campíns-Falcó P (2015) Recent advances of in-tube solid-phase microextraction. TrAC Trends Anal Chem 71:205–213

    Article  CAS  Google Scholar 

  • Mousavi M, Noroozian E, Jalali-Heravi M, Mollahosseini A (2007) Optimization of solid-phase microextraction of volatile phenols in water by a polyaniline-coated Pt-fiber using experimental design. Anal Chim Acta 581:71–77

    Article  CAS  PubMed  Google Scholar 

  • Ngo CL, Le QT, Ngo TT, Nguyen DN, Vu MT (2013) Surface modification and functionalization of carbon nanotube with some organic compounds. Adv Nat Sci Nanosci Nanotechnol 4:035017

    Article  CAS  Google Scholar 

  • Peng C, Jin J, Chen GZ (2007) A comparative study on electrochemical co-deposition and capacitance of composite films of conducting polymers and carbon nanotubes. Electrochim Acta 53:525–537

    Article  CAS  Google Scholar 

  • Piri-Moghadam H, Lendor S, Pawliszyn J (2016) Development of a biocompatible in-tube solid phase microextraction device: a rapid and sensitive approach for direct analysis of single drops of complex matrices. Anal Chem 88:12188–12195

    Article  CAS  PubMed  Google Scholar 

  • Potter DW, Pawliszyn J (1994) Rapid determination of polyaromatic hydrocarbons and polychlorinated biphenyls in water using solid-phase microextraction and GC/MS. Environ Sci Technol 28:298–305

    Article  CAS  PubMed  Google Scholar 

  • Prokůpková G, Holadová K, Poustka J, Hajšlová J (2002) Development of a solid-phase microextraction method for the determination of phthalic acid esters in water. Anal Chim Acta 457:211–223

    Article  Google Scholar 

  • Serôdio P, Nogueira J (2006) Considerations on ultra-trace analysis of phthalates in drinking water. Water Res 40:2572–2582

    Article  CAS  PubMed  Google Scholar 

  • Son HH, Bae S, Lee DS (2012) New needle packed with polydimethylsiloxane having a micro-bore tunnel for headspace in-needle microextraction of aroma components of citrus oils. Anal Chim Acta 751:86–93

    Article  CAS  PubMed  Google Scholar 

  • Tang ZK, Zhang L, Wang N, Zhang XX, Wen GH, Li GD, Wang JN, Chan CT, Sheng P (2001) Superconductivity in 4 angstrom single-walled carbon nanotubes. Science 292:2462–2465

    Article  CAS  PubMed  Google Scholar 

  • Thompson M, Ellison SL, Wood R (2002) Harmonized guidelines for single-laboratory validation of methods of analysis (IUPAC Technical Report). Pure Appl Chem 74:835–855

    Article  CAS  Google Scholar 

  • Wang J, Jiang D, Gu Z, Yan XJ (2006) Multiwalled carbon nanotubes coated fibers for solid-phase microextraction of polybrominated diphenyl ethers in water and milk samples before gas chromatography with electron-capture detection. Chromatogr A 1137:8–14

    Article  CAS  Google Scholar 

  • Wang Y, Li Y, Feng J, Sun C (2008) Polyaniline-based fiber for headspace solid-phase microextraction of substituted benzenes determination in aqueous samples. Anal Chim Acta 619:202–208

    Article  CAS  PubMed  Google Scholar 

  • Wu J, Pawliszyn J (2001) Preparation and applications of polypyrrole films in solid-phase microextraction. J Chromatogr A 909:37–52

    Article  CAS  PubMed  Google Scholar 

  • Zeng Z, Qiu W, Huang Z (2001) Solid-phase microextraction using fused-silica fibers coated with sol-gel-derived hydroxy-crown ether. Anal Chem 73:2429–2436

    Article  CAS  PubMed  Google Scholar 

Download references

Funding

This work was supported by a research grant from Seoul Women’s University (2018).

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Authors and Affiliations

  1. Department of Chemistry, Seoul Women’s University, 621 Hwarang-ro, Nowon-gu, Seoul, 01797, Republic of Korea

    Soyoung Lee, Sunyoung Bae & Dong-Sun Lee

  2. Advanced Analysis Center, Korea Institute of Science and Technology, Seoul, 02792, Republic of Korea

    Jung-Hyeon Yoon

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  1. Soyoung Lee
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  2. Jung-Hyeon Yoon
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  3. Sunyoung Bae
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  4. Dong-Sun Lee
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Correspondence to Sunyoung Bae or Dong-Sun Lee.

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Soyoung Lee declares that she has no conflict of interest. Jung-Hyeon Yoon declares that she has no conflict of interest. Sunyoung Bae declares that she has no conflict of interest. Dong-Sun Lee declares that he has no conflict of interest.

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This article does not contain any studies with human participants or animals performed by any of the authors.

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Lee, S., Yoon, JH., Bae, S. et al. In-needle Microextraction Coupled with Gas Chromatography/Mass Spectrometry for the Analysis of Phthalates Generating from Food Containers. Food Anal. Methods 11, 2767–2777 (2018). https://doi.org/10.1007/s12161-018-1254-6

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  • DOI: https://doi.org/10.1007/s12161-018-1254-6

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