Skip to main content
Log in

Ultrasound-Assisted Extraction Followed by Solid-Phase Extraction Followed by Dispersive Liquid–Liquid Microextraction for the Sensitive Determination of Diazinon and Chlorpyrifos in Rice

  • Published:
Food Analytical Methods Aims and scope Submit manuscript

Abstract

Selectivity of solid-phase extraction (SPE) was combined with the concentration power of dispersive liquid–liquid microextraction (DLLME) to obtain a sensitive, low solvent consumption method for high-performance liquid chromatography determination of diazinon and chlorpyrifos in rice. In this method, rice samples were extracted by ultrasound-assisted extraction followed by SPE. Then, the SPE eluent was used as a disperser solvent in the next dispersive liquid-liquid microextraction step for further purification and enrichment of diazinon and chlorpyrifos. Under the optimal conditions, the linear range was from 5.0 to 250 μg kg−1 for diazinon and from 2.5 to 250 μg kg−1 for chlorpyrifos. Limits of detection of diazinon and chlorpyrifos were 1.5 and 0.7 μg kg−1, respectively. Limits of quantitation of diazinon and chlorpyrifos were 5.5 and 3.0 μg kg−1, respectively. The precisions and recoveries also were investigated by spiking 10 μg kg−1 concentration in rice. The recoveries obtained were over 90 % with relative standard deviation (RSD%) below 9.0 %. The new approach was utilized to successfully detect trace amounts of diazinon and chlorpyrifos in different Iranian rice samples.

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

Access this article

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

Instant access to the full article PDF.

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

Similar content being viewed by others

References

  • Aguilera A, Rodriguez M, Brotons M, Boulaid M, Valverde A (2005) Evaluation of supercritical fluid extraction/aminopropyl solid-phase “in-line” cleanup for analysis of pesticide residues in rice. J Agric Food Chem 53:9374–9382

    Article  CAS  Google Scholar 

  • Bidari A, Zeini Jahromi E, Assadi Y, Milani Hosseini MR (2007) Monitoring of selenium in water samples using dispersive liquid–liquid microextraction followed by iridium-modified tube graphite furnace atomic absorption spectrometry. Microchem J 87:6–12

    Article  CAS  Google Scholar 

  • Cho SK, Abd El-Aty AM, Park YS, Choi JH, Khay S, Kang CK, Park BJ, Kim SJ, Jae-Han Shim JH (2007) A multiresidue method for the analysis of pesticide residues in polished rice (Oryza sativa L.) using accelerated solvent extraction and gas chromatography and confirmation by mass spectrometry. Biomed Chromatogr 21:602–609

    Article  CAS  Google Scholar 

  • Dorea HS, Sobrinho LL (2004) Analysis of pesticide residues in rice using matrix solid-phase dispersion. J Braz Chem Soc 15:690–694

    Article  CAS  Google Scholar 

  • European community Regulation 396/2005, Brussels, Belgium. http://ec.europa.eu/food/plant/protection/pesticides/database-pesticide-en.htm. Accessed 5 June (2009).

  • Farajzadeh MA, Bahram M, Jonsson JA (2007) Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography-diode array detection as an efficient and sensitive technique for determination of antioxidants. Anal Chim Acta 591:69–79

    Article  CAS  Google Scholar 

  • Fattahi N, Samadi S, Assadi Y, Milani Hosseini MR (2007) Solid-phase extraction combined with dispersive liquid-liquid microextraction-ultra preconcentration of chlorophenols in aqueous samples. J Chromatogr A 1169:63–69

    Article  CAS  Google Scholar 

  • Ferrero A, Tinarelli A, Capri E, Karpouzas DG (eds) (2008) Pesticide risk assessment in Rice paddies: theory and practice. Elsevier, Amsterdam, p. 1

    Book  Google Scholar 

  • Fontana AR, Lana NB, Martinez LD, Altamirano JC (2010) Ultrasound-assisted leaching-dispersive solid-phase extraction followed by liquid–liquid microextraction for the determination of polybrominated diphenyl ethers in sediment samples by gas chromatography–tandem mass spectrometry. Talanta 82:359–366

    Article  CAS  Google Scholar 

  • Gonzalez-Curbelo MA, Herrera-Herrera AV, Ravelo-Perez LM, Hernandez-Borges J (2012) Sample-preparation methods for pesticide-residue analysis in cereals and derivatives. Trends Anal Chem 38:32–51

    Article  CAS  Google Scholar 

  • Grande-Martínez A, Arrebola-Liebanas FJ, Martinez-Vidal JL, Hernandez-Torres ME, Garrido-Frenich A (2016) Optimization and validation of a multiresidue pesticide method in rice and wheat flour by modified QuEChERS and GC–MS/MS. Food Anal Methods 9:548–563

    Article  Google Scholar 

  • Henriques Alves AC, Boavida Gonçalves MMP, Serrano Bernardo MM, Mendes BS (2011) Determination of organophosphorous pesticides in the ppq range using a simple solid-phase extraction method combined with dispersive liquid–liquid microextraction. J Sep Sci 34:2475–2481

    Article  Google Scholar 

  • Herrmann SS, Poulsen ME (2015) Clean-up of cereal extracts for gas chromatography–tandem quadrupole mass spectrometry pesticide residues analysis using primary secondary amine and C18. J Chromatogr A 1423:47–53

    Article  CAS  Google Scholar 

  • Kaihara A, Yoshii K, Tsumura Y, Ishimitsu S, Tonogai Y (2002) Multi-residue analysis of 18 pesticides in fresh fruits, vegetables and rice by supercritical fluid extraction and liquid chromatography-electrospray ionization mass spectrometry. J Health Sci 48:173–178

    Article  CAS  Google Scholar 

  • Katsumata H, Matsumoto T, Kaneco S, Suzuki T, Ohta K (2008) Preconcentration of diazinon using multiwalled carbon nanotubes as solid-phase extraction adsorbents. Microchem J 88:82–86

    Article  CAS  Google Scholar 

  • Lee SJ, Park HJ, Kim W, Jin JS, El-Aty AMA, Shim JH, Shin SC (2009) Multiresidue analysis of 47 pesticides in cooked wheat flour and polished rice by liquid chromatography with tandem mass spectrometry. Biomed Chromatogr 23:434–442

    Article  CAS  Google Scholar 

  • Liu X, Li J, Zhao Z, Zhang W, Lin K, Huang C, Wang X (2009) Solid-phase extraction combined with dispersive liquid–liquid microextraction for the determination for polybrominated diphenyl ethers in different environmental matrices. J Chromatogr A 1216:2220–2226

    Article  CAS  Google Scholar 

  • Pareja L, Fernandez-Alba AR, Cesio V, Heinzen H (2011) Analytical methods for pesticide residues in rice. Trends Anal Chem 30:270–291

    Article  CAS  Google Scholar 

  • Pengyan L, Qingxue L, Yusong M, Jinwei L, Xuan J (2006a) Analysis of pesticide multiresidues in rice by gas chromatography-mass spectrometry coupled with solid phase extraction. Chin J Chromatogr 24:228–234

    Article  Google Scholar 

  • Pengyan L, Qingxue L, Yusong M, Jinwei L, Xuan J, Chin J (2006b) Analysis of pesticide multiresidues in rice by gas chromatography-mass spectrometry coupled with solid phase extraction. J Chromatogr A 24:228–238

    Google Scholar 

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

  • Rezaee M, Yamini Y, Shariati S, Esrafili A, Shamsipur M (2009) Dispersive liquid-liquid microextraction combined with high-performance liquid chromatography-UV detection as a very simple, rapid and sensitive method for the determination of bisphenol A in water samples. J Chromatogr A 1216:1511–1514

    Article  CAS  Google Scholar 

  • Rezaee M, Yamini Y, Faraji M (2010) Evolution of dispersive liquid-liquid microextraction. J Chromatogr A 1217:2342–2357

    Article  CAS  Google Scholar 

  • Shokoufi N, Shemirani F, Assadi Y (2007) Fiber optic-linear array detection spectrophotometry in combination with dispersive liquid–liquid microextraction for simultaneous preconcentration and determination of palladium and cobalt. Anal Chim Acta 597:349–356

    Article  CAS  Google Scholar 

  • Skopec ZV, Clark R, Harvey PMA, Wells RJ (1993) Analysis of organophosphorus pesticides in rice by supercritical fluid extraction and quantitation using an atomic emission detector. J Chromatogr Sci 31:445–449

    Article  CAS  Google Scholar 

  • Soodi M, Garshasbi A, Eskandari S (2012) Development a HPLC method for simultaneous determination of Azinphose methyl, Diazinon, Phosalone and Chlorpyrifos residues in fruit. J Pharm Health Sci 4:79–87

    Google Scholar 

  • Tsochatzis ED, Menkissoglu-Spiroudi U, Karpouzas DG, Tzimou-Tsitouridou R (2010) A multi-residue method for pesticide residue analysis in rice grains using matrix solid-phase dispersion extraction and high-performance liquid chromatography-diode array detection. Anal Bioanal Chem 397:2181–2190

    Article  CAS  Google Scholar 

  • Uddin R, Iqbal S, Farhanullah Khan M, Parveen Z, Ahmed M, Abbas M (2011) Determination of pesticide residues in rice grain by solvent extraction, column cleanup, and gas chromatography-electron capture detection. Bull Environ Contam Toxicol 86:83–89

    Article  CAS  Google Scholar 

  • Valverde A, Aguilera A, Rodriguez M, Brotons M (2009) Evaluation of a multiresidue method for pesticides in cereals using supercritical fluid extraction and gas chromatographic detection. J Environ Sci Health Part B 44:204–213

    Article  CAS  Google Scholar 

  • Yamini Y, Rezaee M, Khanchi A, Faraji M, Saleh A (2010) Dispersive liquid–liquid microextraction based on the solidification of floating organic drop followed by inductively coupled plasma-optical emission spectrometry as a fast technique for the simultaneous determination of heavy metals. J Chromatogr A 1217:2358–2364

    Article  CAS  Google Scholar 

  • Zhang WG, Chu XG, Cai HX, An J, Li CJ (2006) Simultaneous determination of 109 pesticides in unpolished rice by a combination of gel permeation chromatography and Florisil column purification, and gas chromatography/mass spectrometry. Rapid Commun Mass Spectrom 20:609–617

    Article  CAS  Google Scholar 

  • Zhao EC, Zhao WT, Han LJ, Jiang SR, Zhou ZQ (2007) Application of dispersive liquid–liquid microextraction for the analysis of organophosphorus pesticides in watermelon and cucumber. J Chromatogr A 1175:137–140

    Article  CAS  Google Scholar 

Download references

Acknowledgment

Financial support from Yadegar -e- Imam Khomeini (RAH) Shahre Rey Branch, Islamic Azad University, Tehran, Iran for the support during the period of this research is gratefully acknowledged.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Faezeh Khalilian.

Ethics declarations

Funding

There is no funding for this study.

Conflict of Interest

No conflict exists; author Faezeh khalilian declares that she has no conflict of interest. Author Mohammad Rezaee declares that he 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.

Informed Consent

No humans are involved in this study.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Khalilian, F., Rezaee, M. Ultrasound-Assisted Extraction Followed by Solid-Phase Extraction Followed by Dispersive Liquid–Liquid Microextraction for the Sensitive Determination of Diazinon and Chlorpyrifos in Rice. Food Anal. Methods 10, 885–891 (2017). https://doi.org/10.1007/s12161-016-0653-9

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s12161-016-0653-9

Keywords

Navigation