Skip to main content
SpringerLink
Log in

Development of an Efficient Sample Preparation Method Based on Homogeneous Liquid-Liquid Extraction Combined with Dispersive Liquid-Liquid Microextraction Solidification of Floating Organic Drop for Trace Analysis of Pesticide Residues in Fruit and Fruit Juice Samples

  • Published:
Food Analytical Methods Aims and scope Submit manuscript

Abstract

In this study, a simple and reliable sample preparation method based on an efficient version of homogeneous liquid-liquid extraction combined with dispersive liquid-liquid microextraction solidification of floating organic drop has been introduced to analyze some pesticide residues in fruit and fruit juice samples with gas chromatography-flame ionization detection. Under the optimum experimental conditions, limits of detection and quantification were in the ranges of 0.20–0.60 and 0.66–2.0 μg L−1, respectively. The repeatability of the method was good and the relative standard deviations were less than 7 % for intra- (n = 6) and inter-day (n = 4) precisions at a concentration of 50 μg L−1 of each analyte. High enrichment factors (3265–3728) and extraction recoveries (82–93 %) were obtained. Finally, the method was applied for determination of pesticides in the selected samples and chlorpyrifos was found in strawberry at ng g−1 concentration. Furthermore, no filtration was used in the cases of the fruit samples.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Scheme 1
Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7

Similar content being viewed by others

Abbreviations

DLLME:

Dispersive liquid-liquid microextraction

EF:

Enrichment factor

ER:

Extraction recovery

FID:

Flame ionization detection

GC:

Gas chromatography

HLLE:

Homogeneous liquid-liquid extraction

LLE:

Liquid-liquid extraction

LOD:

Limit of detection

LPME:

Liquid-phase microextraction

LOQ:

Limit of quantification

MS:

Mass spectrometry

RSD:

Relative standard deviation

SFO:

Solidification of floating organic drop

SPE:

Solid-phase extraction

References

  • Amini T, Hashemi P (2018) Preconcentration and GC–MS determination of caffeine in tea and coffee using homogeneous liquid–liquid microextraction based on solvents volume ratio alteration. J Chromatogr B 1092:252–257

    Article  CAS  Google Scholar 

  • Anthemidis AN, Adam IS (2009) Development of on-line single-drop micro-extraction sequential injection system for electrothermal atomic absorption spectrometric determination of trace metals. Anal Chim Acta 632:216–220

    Article  CAS  Google Scholar 

  • Chen H, Chen R, Li S (2010) Low-density extraction solvent-based solvent terminated dispersive liquid–liquid microextraction combined with gas chromatography-tandem mass spectrometry for the determination of carbamate pesticides in water samples. J Chromatogr A 1217:1244–1248

    Article  CAS  Google Scholar 

  • Costa LG, Giordano G, Guizzetti M, Vitalone A (2008) Neurotoxicity of pesticides: a brief review. Front Biosci 13:1240–1249

    Article  CAS  Google Scholar 

  • Djozan D, Assadi Y (2004) Modified pencil lead as a new fiber for solid-phase microextraction. Chromatographia 60:313–317

    CAS  Google Scholar 

  • Ebrahimzadeh H, Yamini Y, Kamarei F, Shariati S (2007) Homogeneous liquid–liquid extraction of trace amounts of mononitrotoluenes from waste water samples. Anal Chim Acta 594:93–100

    Article  CAS  Google Scholar 

  • 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 35:534–540

    Article  CAS  Google Scholar 

  • Farajzadeh MA, Mogaddam MRA, Aghdam SR, Nouri N, Bamorrowat M (2016) Application of elevated temperature-dispersive liquid-liquid microextraction for determination of organophosphorus pesticides residues in aqueous samples followed by gas chromatography-flame ionization detection. Food Chem 212:198–204

    Article  CAS  Google Scholar 

  • Farajzadeh MA, Alavian AS, Dabbagh MS (2018) Application of vortex-assisted liquid–liquid microextraction based on solidification of floating organic droplets for determination of some pesticides in fruit juice samples. Anal Methods 10:5842–5850

    Article  CAS  Google Scholar 

  • Gao Z, Ma X (2011) Speciation analysis of mercury in water samples using dispersive liquid–liquid microextraction combined with high-performance liquid chromatography. Anal Chim Acta 702:50–55

    Article  CAS  Google Scholar 

  • Gao Y, Sun P (2018) Determination of five pyrethroid pesticides residue in liquid milk by gas chromatography using multi-walled carbon nanotubes as dispersion solid phase extraction sorbent. Acta Chromatogr 30:141–146

    Article  CAS  Google Scholar 

  • Ghiasvand A, Shadabi S, Mohagheghzadeh E, Hashemi P (2005) Homogeneous liquid–liquid extraction method for the selective separation and preconcentration of ultra trace molybdenum. Talanta 66:912–916

    Article  CAS  Google Scholar 

  • Khalili-Zanjani MR, Yamini Y, Yazdanfar N, Shariati S (2008) Extraction and determination of organophosphorus pesticides in water samples by a new liquid phase microextraction–gas chromatography–flame photometric detection. Anal Chim Acta 606:202–208

    Article  CAS  Google Scholar 

  • Khan DA, Bhatti MM, Khan FA, Naqvi ST, Karam A (2008) Adverse effects of pesticides residues on biochemical markers in Pakistani tobacco farmers. Int J Clin Exp Med 1:274

    CAS  PubMed  PubMed Central  Google Scholar 

  • Kokosa JM, Przyjazny A, Jeannot M (2009) Solvent microextraction: theory and practice. John Wiley & Sons

  • Li S, Gao P, Zhang J, Li Y, Peng B, Gao H, Zhou W (2012) Sequential dispersive liquid–liquid microextraction for the determination of aryloxyphenoxy-propionate herbicides in water. J Sep Sci 35:3389–3395

    Article  CAS  Google Scholar 

  • Miró M, Estela JM, Cerdà V (2005) Recent advances in on-line solvent extraction exploiting flow injection/sequential injection analysis. Curr Anal Chem 1:329–343

    Article  Google Scholar 

  • Murata K, Yokoyama Y, Ikeda S (1972) Homogeneous liquid-liquid extraction method. Extraction of iron (III) thenoyltrifluoroacetonate by propylene carbonate. Anal Chem 44:805–810

    Article  CAS  Google Scholar 

  • Nieto A, Borrull F, Pocurull E, Marcé RM (2010) Pressurized liquid extraction: a useful technique to extract pharmaceuticals and personal-care products from sewage sludge. TrAC Trends Anal Chem 29:752–764

    Article  CAS  Google Scholar 

  • Ojeda CB, Rojas FS (2009) Separation and preconcentration by dispersive liquid–liquid microextraction procedure: a review. Chromatographia 69:1149–1159

    Article  Google Scholar 

  • Oshite S, Igarashi S (2001) Homogeneous liquid-liquid extraction as preconcentration method using water/tetrabutylammonium bromide/chloroform ternary component system and its application to the flame-less atomic absorption spectrometry. In: Analytical Sciences/Supplements Proceedings of IUPAC International Congress on Analytical Sciences. JSAC, pp 1329–1331

  • Paleologos EK, Giokas DL, Karayannis MI (2005) Micelle-mediated separation and cloud-point extraction. TrAC Trends Anal Chem 24:426–436

    Article  CAS  Google Scholar 

  • Pirsaheb M, Fattahi N, Shamsipur M (2013) Determination of organophosphorous pesticides in summer crops using ultrasound-assisted solvent extraction followed by dispersive liquid–liquid microextraction based on the solidification of floating organic drop. Food Control 34:378–385

    Article  CAS  Google Scholar 

  • Płotka-Wasylka J, Szczepańska N, de la Guardia M, Namieśnik J (2015) Miniaturized solid-phase extraction techniques. TrAC Trends Anal Chem 73:19–38

    Article  Google Scholar 

  • Rastegarzadeh S, Pourreza N, Larki A (2014) Dispersive liquid–liquid microextraction for the microvolume spectrophotometric determination of bismuth in pharmaceutical and human serum samples. Anal Methods 6:3500–3505

    Article  CAS  Google Scholar 

  • Rezaee M, Assadi Y, Hosseini M-RM, Aghaee E, Ahmadi F, Berijani S (2006) Determination of organic compounds in water using dispersive liquid–liquid microextraction. J Chromatogr A 1116:1–9

    Article  CAS  Google Scholar 

  • Sarafraz-Yazdi A, Assadi H, Wan Ibrahim WA (2012) Determination of triazole fungicides using hollow fiber liquid phase microextraction prior to gas chromatography–mass spectrometry analysis. Ind Eng Chem Res 51:3101–3107

    Article  CAS  Google Scholar 

  • Takahashi A, Yamaguchi H, Igarashi S (1997) Homogeneous liquid-liquid extraction method for some kinds of high-valence metal ions using desferrioxamine B. Bunseki Kagaku 46:55–58

    Article  CAS  Google Scholar 

  • Takahashi A, Ueki Y, Igarashi S (1999) Homogeneous liquid–liquid extraction of uranium (VI) from acetate aqueous solution. Anal Chim Acta 387:71–75

    Article  CAS  Google Scholar 

  • Tobiszewski M, Mechlińska A, Namieśnik J (2010) Green analytical chemistry—theory and practice. Chem Soc Rev 39:2869–2878

    Article  CAS  Google Scholar 

  • Zahedi MM, Rahimi-Nasrabadi M, Pourmortazavi SM, Koohbijari GRF, Shamsi J, Payravi M (2012) Emulsification-based dispersive liquid microextraction and HPLC determination of carbazole-based explosives. Microchim Acta 179:57–64

    Article  CAS  Google Scholar 

  • Zanjani MRK, Yamini Y, Shariati S, Jönsson JÅ (2007) A new liquid-phase microextraction method based on solidification of floating organic drop. Anal Chim Acta 585:286–293

    Article  Google Scholar 

  • Zhou Q, Liu J, Cai Y, Liu G, Jiang G (2003) Micro-porous membrane liquid–liquid extraction as an enrichment step prior to nonaqueous capillary electrophoresis determination of sulfonylurea herbicides. Microchem J 74:157–163

    Article  CAS  Google Scholar 

Download references

Acknowledgments

The financial support from University of Tabriz is acknowledged.

Funding

Mir Ali Farajzadeh has received research grants from University of Tabriz.

Author information

Authors and Affiliations

  1. Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran

    Mir Ali Farajzadeh, Ali Sadeghi Alavian & Masoumeh Sattari Dabbagh

  2. Engineering Faculty, Near East University, North Cyprus, 99138, Nicosia, Mersin 10, Turkey

    Mir Ali Farajzadeh

Authors
  1. Mir Ali Farajzadeh
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Ali Sadeghi Alavian
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Masoumeh Sattari Dabbagh
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Mir Ali Farajzadeh.

Ethics declarations

Conflict of Interest

Mir Ali Farajzadeh declares that he has no conflict of interest. Ali Sadeghi Alavian declares that he has no conflict of interest. Masoumeh Sattari Dabbagh declares that she has no conflict of interest.

Ethical Approval

This article does not contain any studies with human or animals.

Additional information

Publisher’s Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Farajzadeh, M.A., Sadeghi Alavian, A. & Sattari Dabbagh, M. Development of an Efficient Sample Preparation Method Based on Homogeneous Liquid-Liquid Extraction Combined with Dispersive Liquid-Liquid Microextraction Solidification of Floating Organic Drop for Trace Analysis of Pesticide Residues in Fruit and Fruit Juice Samples. Food Anal. Methods 12, 2730–2741 (2019). https://doi.org/10.1007/s12161-019-01628-y

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s12161-019-01628-y

Keywords

Search

Navigation