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In-Tube Ultrasound Assisted Dispersive Solid–Liquid Microextraction Based on Self-Assembly and Solidification of an Alkanol-Based Floating Organic Droplet for Determination of Pyrethroid Insecticides in Chrysanthemum

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Abstract

A new in-tube pretreatment method based on ultrasound assisted dispersive solid–liquid microextraction using self-assembly and solidification of an alkanol-based floating organic droplet was developed for the determination of eight pyrethroid insecticides in chrysanthemum by gas chromatography with electron capture detection. This method fully utilized the restricted access property of a 1-decanol/acetonitrile mixture for effective extraction of the analytes from chrysanthemum under ultrasonication, and the self-assembly and coacervation process of 1-decanol by adding water. The 1-decanol phase aggregated and floated on the surface, solidified in an ice bath, and thus was easily collected. For the first time, extraction, separation and preconcentration were combined in a tube, not requiring stepwise preparation for a solid matrix. The recoveries ranged from 75 to 104% with the relative standard deviations of < 8%. The limits of quantification were in the range of 0.15–1.5 µg kg− 1 up to 52-fold compared with the conventional QuEChERS-based, SPE, and solid–liquid dispersive microextraction methods. The results demonstrated that the proposed method was time-saving, sensitive, and environmentally friendly for pyrethroids analysis in chrysanthemum.

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References

  1. Xue JY, Chen XC, Jiang WQ, Liu FM, Li HC (2015) Rapid and sensitive analysis of nine fungicide residues in chrysanthemum by matrix extraction-vortex-assisted dispersive liquid–liquid microextraction. J Chromatogr B 975:9–17

    Article  CAS  Google Scholar 

  2. Xue JY, Xu YJ, Liu FM, Xue J, Li HC, Peng W (2013) Comparison of different sample pre-treatments for multi-residue analysis of organochlorine and pyrethroid pesticides in chrysanthemum by gas chromatography with electron capture detection. J Sep Sci 36:1311–1316

    Article  CAS  PubMed  Google Scholar 

  3. Xue J, Hao LL, Peng F (2008) Residues of 18 organochlorine pesticides in 30 traditional Chinese medicines. Chemosphere 71:1051–1055

    Article  CAS  PubMed  Google Scholar 

  4. Xue JY, Li HC, Liu FM, Xue J, Chen XC, Zhan J (2014) Transfer of difenoconazole and azoxystrobin residues from chrysanthemum flower tea to its infusion. Food Addit Contam Part A 31:666–675

    Article  CAS  Google Scholar 

  5. Chen HP, Gao GW, Liu PX, Pan ML, Chai YF, Liu X, Lu CY (2017) Development and validation of an ultra performance liquid chromatography exactive orbitrap mass spectrometry for the determination of fipronil and its metabolites in tea and chrysanthemum. Food Chem 246:328–334

    Article  CAS  PubMed  Google Scholar 

  6. Petrarca MH, Ccanccapa-Cartagena A, Masiá A, Godoy HT, Picó Y (2017) Comparison of green sample preparation techniques in the analysis of pyrethrins and pyrethroids in baby food by liquid chromatography-tandem mass spectrometry. J Chromatogr A 1497:28–37

    Article  CAS  PubMed  Google Scholar 

  7. Ccanccapa-Cartagena A, Masiá A, Picó Y (2017) Simultaneous determination of pyrethroids and pyrethrins by dispersive liquid-liquid microextraction and liquid chromatography triple quadrupole mass spectrometry in environmental samples. Anal Bioanal Chem 409:4787–4799

    Article  CAS  PubMed  Google Scholar 

  8. Amde M, Tan ZQ, Liu R, Liu JF (2015) Nanofluid of zinc oxide nanoparticles in ionic liquid for single drop liquid microextraction of fungicides in environmental waters prior to high performance liquid chromatographic analysis. J Chromatogr A 1395:7–15

    Article  CAS  PubMed  Google Scholar 

  9. Wang HZ, Hu L, Li WZ, Yang XL, Lu RH, Zhang SB, Zhou WF, Gao HX, Li J (2017) In-syringe dispersive liquid-liquid microextraction based on the solidification of ionic liquids for the determination of benzoylurea insecticides in water and tea beverage samples. Talanta 162:625–633

    Article  CAS  PubMed  Google Scholar 

  10. Zhang Y, Zhang X, Jiao B (2014) Determination of ten pyrethroids in various fruit juices: comparison of dispersive liquid-liquid microextraction sample preparation and QuEChERS method combined with dispersive liquid-liquid microextraction. Food Chem 159:367–373

    Article  CAS  PubMed  Google Scholar 

  11. Xue JY, Li HC, Liu FM, Jiang WQ, Chen XC (2014) Determination of strobilurin fungicides in cotton seed by combination of acetonitrile extraction and dispersive liquid-liquid microextraction coupled with gas chromatography. J Sep Sci 37:845–852

    Article  CAS  PubMed  Google Scholar 

  12. Samadi S, Sereshti H, Assadi Y (2012) Ultra-preconcentration and determination of thirteen organophosphorus pesticides in water samples using solid-phase extraction followed by dispersive liquid-liquid microextraction and gas chromatography with flame photometric detection. J Chromatogr A 1219:61–65

    Article  CAS  PubMed  Google Scholar 

  13. Jowkarderis M, Raofie F (2012) Optimization of supercritical fluid extraction combined with dispersive liquid-liquid microextraction as an efficient sample preparation method for determination of 4-nitrotoluene and 3-nitrotoluene in a complex matrix. Talanta 88:50–53

    Article  CAS  PubMed  Google Scholar 

  14. Farajzadeh MA, Djozan D, Nouri N, Bamorowat M, Shalamzari MS (2010) Coupling stir bar sorptive extraction-dispersive liquid-liquid microextraction for pre-concentration of triazole pesticides from aqueous samples followed by GC-FID and GC-MS determinations. J Sep Sci 33:1816–1828

    Article  CAS  PubMed  Google Scholar 

  15. Bazregar M, Rajabi M, Yamini Y, Saffarzadeh Z, Asghari A (2016) Tandem dispersive liquid-liquid microextraction as an efficient method for determination of basic drugs in complicated matrices. J Chromatogr A 1429:13–21

    Article  CAS  PubMed  Google Scholar 

  16. Ballesteros-Gómez A, Rubio S (2012) Environment-responsive alkanol-based supramolecular solvents: Characterization and potential as restricted access property and mixed-mode extractants. Anal Chem 84:342–349

    Article  CAS  PubMed  Google Scholar 

  17. Ballesteros-Gómez A, Lunar L, Sicilia MD, Rubio S (2018) Hyphenating supramolecular solvents and liquid chromatography: tips for efficient extraction and reliable determination of organics. Chromatographia. https://doi.org/10.1007/s10337-018-3614-1

    Article  Google Scholar 

  18. Saraji M, Boroujeni MK (2014) Recent developments in dispersive liquid-liquid microextraction. Anal Bioanal Chem 406:2027–2066

    Article  CAS  PubMed  Google Scholar 

  19. Ho Y-M, Tsoi Y-K, Leung KS-Y (2013) Highly sensitive and selective organophosphate screening in twelve commodities of fruits, vegetables and herbal medicines by dispersive liquid–liquid microextraction. Anal Chim Acta 775:58–66

    Article  CAS  PubMed  Google Scholar 

  20. Vera-Avila LE, Rojo-Portillo T, Ovarrubias-Herrera R, Peña-Alvarez A (2013) Capabilities and limitations of dispersive liquid-liquid microextraction with solidification of floating organic drop for the extraction of organic pollutants from water samples. Anal Chim Acta 805:60–69

    Article  CAS  PubMed  Google Scholar 

  21. Bolzan CM, Caldas SS, Guimarães BS, Primel EG (2016) Dispersive liquid-liquid microextraction based on solidification of floating organic droplet for the determination of triazine and triazoles in mineral water samples. J Sep Sci 39:3410–3417

    Article  CAS  PubMed  Google Scholar 

  22. Pirsaheb M, Fattahi N, Shamsipur M, Khodadadi T (2013) Application of dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous determination of alachlor and atrazine in aqueous samples. J Sep Sci 36:684–689

    Article  CAS  PubMed  Google Scholar 

  23. Sanagi MM, Abbas HH, Ibrahim WAW, Aboul-Enien HY (2012) Dispersive liquid-liquid microextraction method based on solidification of floating organic droplet for the determination of triazine herbicides in water and sugarcane samples. Food Chem 133:557–562

    Article  CAS  PubMed  Google Scholar 

  24. Lima DL, Silva CP, Otero M, Esteves VI (2013) Low cost methodology for estrogens monitoring in water samples using dispersive liquid-liquid microextraction and HPLC with fluorescence detection. Talanta 115:980–985

    Article  CAS  PubMed  Google Scholar 

  25. Farajzadeh MA, Afshar Mogaddam MR, 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 Chemi 212:198–204

    Article  CAS  Google Scholar 

  26. Mirparizi E, Rajabi M, Bazregar M, Asghari A (2017) Centrifugeless dispersive liquid-liquid microextraction based on salting-out phenomenon as an efficient method for determination of phenolic compounds in environmental samples. Anal Bioanal Chem 409:3007–3016

    Article  CAS  PubMed  Google Scholar 

  27. Chen PS, Haung WY, Huang SD (2014) Analysis of triazine herbicides using an up-and- down-shaker-assisted dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry. J Chromatogr B 955–956:116–123

    Article  CAS  Google Scholar 

  28. Lin ZB, Li JL, Zhang XY, Qiu MH, Huang ZB, Rao YL (2017) Ultrasound-assisted dispersive liquid-liquid microextraction for the determination of seven recreational drugs in human whole blood using gas chromatography-mass spectrometry. J Chromatogr B 1046:177–184

    Article  CAS  Google Scholar 

  29. Ghazaghi M, Mousavi HZ, Shirkhanloo H, Rashidi A (2017) Stirring-controlled solidified floating solid-liquid drop microextraction as a new solid phase-enhanced liquid-phase microextraction method by exploiting magnetic carbon nanotube-nickel hybrid. Anal Chim Acta 951:78–88

    Article  CAS  PubMed  Google Scholar 

  30. Wang HZ, Hu L, Liu XY, Yin SJ, Lu RH, Zhang SB, Zhou WF, Gao HX (2017) Deep eutectic solvent-based ultrasound-assisted dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the determination of ultraviolet filters in water samples. J Chromatogr A 1516:1–8

    Article  CAS  PubMed  Google Scholar 

  31. Xue JY, Li HC, Liu FM, Jiang WQ, Hou F (2016) Vortex-assisted matrix solid-liquid dispersive microextraction for the analysis of triazole fungicides in cotton seed and honeysuckle by gas chromatography. Food Chem 196:867–876

    Article  CAS  PubMed  Google Scholar 

  32. Qi XY (2010) Development of a matrix solid-phase dispersion-sonication extraction method for the determination of fungicides residues in ginseng extract. Food Chem 121:758–762

    Article  CAS  Google Scholar 

  33. Quan C, Shang YG, Li SF, Tang SK, Huang T, Fang X (2010) Kinetic study of supercritical fluid extraction of organochlorine pesticides from ginseng by Simulink simulation. J Taiwan Inst Chem Eng 41:44–48

    Article  CAS  Google Scholar 

  34. Huang XH, Zhao XH, Lu XT, Tian HP, Xu AJ, Liu Y, Jian Z (2014) Simultaneous determination of 50 residual pesticides in flos chrysanthemi using accelerated solvent extraction and gas chromatography. J Chromatogr B 967:1–7

    Article  CAS  Google Scholar 

Download references

Acknowledgements

This work was partly supported by the National Key Research and Development Program of China (2016YFD0200201), the National Natural Science Foundation of China (41807490), the Natural Science Research Project of High Education of Anhui (KJ2018A0128), and the University Youth Science Foundation of Anhui Agricultural University (2017zd04).

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Correspondence to Rimao Hua.

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Author Jiaying Xue declares that she has no conflict of interest. Author Dong Zhang declares that he has no conflict of interest. Author Xiangwei Wu declares that he has no conflict of interest. Author Dandan Pan declares that she has no conflict of interest. Author Rimao Hua declares that he has no conflict of interest.

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Xue, J., Zhang, D., Wu, X. et al. In-Tube Ultrasound Assisted Dispersive Solid–Liquid Microextraction Based on Self-Assembly and Solidification of an Alkanol-Based Floating Organic Droplet for Determination of Pyrethroid Insecticides in Chrysanthemum. Chromatographia 82, 695–704 (2019). https://doi.org/10.1007/s10337-018-3678-y

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  • DOI: https://doi.org/10.1007/s10337-018-3678-y

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