Skip to main content
Log in

Dispersive liquid-liquid microextraction of phenolic compounds using solidified floating organic droplets, and their determination by HPLC

  • Original Paper
  • Published:
Microchimica Acta Aims and scope Submit manuscript

Abstract

We have developed a simple and efficient method for dispersive liquid-liquid microextraction of 4-nitrophenol, 2-naphthol and bisphenol A in real water samples. It is making use of solidified floating organic droplets of 1-dodecanol which has low density and a proper melting point. The type and volume of extraction solvent and dispersive solvent, the effect of salts, pH value and extraction time were optimized and resulted in enrichment factors of 84 for 4-nitrophenol, 123 for 2-naphthol, and 97 for bisphenol A. The limits of detection by HPLC are 1.50, 0.10 and 1.02 ng · mL−1, respectively. Excellent linearity is observed in the concentration range from 10 to 800 ng · mL−1, with coefficients of correlation ranging from 0.9988 to 0.9999. The relative standard deviations (for n = 5) are from 3.2 to 5.3 %, and relative recoveries for the three phenols in tap, river and spring water range from 85.0 to 105.0 %, 98.3 to 110.0 %, and 98.6 to 109.0 %, respectively.

Chromatograms of river water blank (b) and spiked river water (a, 500 ng ∙ mL−1) analyzed with DLLME-SFO-HPLC. Peak identification: (1) p-nitrophenol; (2) 2-naphthol; (3) bisphenol A. Liquid-liquid microextraction method based on solidification of floating organic droplet (DLLME-SFO) has a high enrichment factor (84, 123and 97), acceptable relative recovery (85.0 %–110.0 %), good repeatability (5.27 %, 3.54 % and 3.16 %) and a wide linear range (10–800 ng · mL−1) for the determination of p-nitrophenol, 2-naphthol and bisphenol A.

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

Similar content being viewed by others

References

  1. Ou JJ, Hu LH, Hu LG, Li X, Zou HF (2006) Determination of phenolic compounds in river water with on-line coupling bisphenol A imprinted monolithic precolumn with high performance liquid chromatography. Talanta 69:1001–1006

    Article  CAS  Google Scholar 

  2. Zhou FR, Li XJ, Zeng ZR (2005) Determination of phenolic compounds in wastewater samples using a novel fiber by solid-phase microextraction coupled to gas chromatography. Anal Chim Acta 538:63–70

    Article  CAS  Google Scholar 

  3. He Y, Vargas A, Kang YJ (2007) Headspace liquid-phase microextraction of methamphetamine and amphetamine in urine by an aqueous drop. Anal Chim Acta 589:225–230

    Article  CAS  Google Scholar 

  4. Faraji H, Tehrani MS, Tehrani SW (2009) Pre-concentration of phenolic compounds in water samples by novel liquid-liquid microextraction and determination by gas chromatography–mass spectrometry. J Chromatogr A 1216:8569–8574

    Article  CAS  Google Scholar 

  5. Caro E, Marce RM, Cormack PAG (2003) On-line solid-phase extraction with molecularly imprinted polymers to selectively extract substituted 4-chlorophenols and 4-nitrophenol from water. J Chromatogr A 995:233–238

    Article  CAS  Google Scholar 

  6. Yao GY, Guan WN, Xu F, Wang H, Guan F (2008) Analysis of phenolic compounds in aqueous samples by gas chromatography coupled with headspace solid-phase microextraction using poly (phthalazine ether sulfone ketone) coated fiber. Chin J Chromatogr 26:590–594

    CAS  Google Scholar 

  7. Hua XX, Yin Y, Hu YL, Ke LG (2007) Determination of trace phenolic compounds in water samples by liquid-liquid-liquid microextraction coupled with HPLC. J Instr Anal 26:797–801

    Google Scholar 

  8. Nerín C, Philo MR, Salafranca J, Castle L (2002) Determination of bisphenol-type contaminants from food packaging materials in aqueous foods by solid-phase microextraction-high-performance liquid chromatography. J Chromatogr A 963:375–380

    Article  Google Scholar 

  9. Sanagi MM, Miskam M, Wan Ibrahim WA, Hermawan D, Aboul-Enein HY (2010) Determination of partition coefficient and analysis of nitrophenols by three-phase liquid-phase microextraction coupled with capillary electrophoresis. J Sep Sci 387:2911–2915

    Google Scholar 

  10. Wu Y, Hu B, Hou Y (2008) Headspace single drop and hollow fiber liquid phase microextractions for HPLC determination of phenols. J Sep Sci 31:3772–3781

    Article  CAS  Google Scholar 

  11. Xia J, Xiang B, Zhang W (2008) Determination of metacrate in water samples using dispersive liquid–liquid microextraction and HPLC with the aid of response surface methodology and experimental design. Anal Chim Acta 625:28–34

    Article  CAS  Google Scholar 

  12. Melwanki MB, Fuh MR (2008) Partitioned dispersive liquid-liquid microextraction: an approach for polar orgnic compounds extraction from aqueous samples. J Chromatogr A 1207:24–28

    Article  CAS  Google Scholar 

  13. Yazdi AS, Amiri A (2010) Liquid-phase microextraction. Trends Anal Chem 29:1–14

    Article  Google Scholar 

  14. He LJ, Luo XL, Xie HX, Wang CJ, Jiang XM, Lu K (2009) Ionic liquid-based dispersive liquid-liquid microextraction followed high-performance liquid chromatography for the determination of organophosphorus pesticides in water sample. Anal Chim Acta 655:52–59

    Article  CAS  Google Scholar 

  15. Han D, Row KH (2012) Trends in liquid-phase microextraction, and its application to environmental and biological samples. Microchim Acta 176:1–22

    Article  CAS  Google Scholar 

  16. Rezaee M, Assadi Y, Milani MR, 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 

  17. Jiang XY, Zhang H, Chen XQ (2011) Determination of phenolic compounds in water samples by HPLC following ionic liquid dispersive liquid-liquid microextraction and cold-induced aggregation. Microchim Acta 175:341–346

    Google Scholar 

  18. Berijani S, Assadi Y, Anbia M, Hosseini M-RM, Aghaee E (2006) Dispersive liquid-liquid microextraction combined with gas chromatography-flame photometric detection: Very simple, rapid and sensitive method for the determination of organophosphorus pesticides in water. J Chromatogr A 1123:1–9

    Google Scholar 

  19. Mohsen Z, Mohammad RG, Parviz N (2010) Dispersive liquid-liquid microextraction followed by spectrofluorimetry as a simple and accurate technique for determination of thiamine (vitamin B-1). Microchim Acta 168:317–324

    Article  Google Scholar 

  20. Zhu HY, Cao ZB, Mou XG (2006) Application of room temperature ionic liquids. Chem Prod Technol 13:40–42

    CAS  Google Scholar 

  21. Xu AM, Sun XQ, She ZB, Chen J, Li DQ (2006) The recent development of room temperature ionic liquids in separation science and technology. J Mol Sci 22:287–293

    Google Scholar 

  22. Liu HQ, Zhang MH, Wang XD, Zou YJ, Wang WW, Ma MP, Li YY, Wang HL (2012) Extraction and determination of polybrominated diphenyl ethers in water and urine samples using solidified floating organic drop microextraction along with high performance liquid chromatography. Microchim Acta 176:303–309

    Article  CAS  Google Scholar 

  23. 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 

  24. Somayeh T, Mohammad AT (2011) New method for microextraction of ultra trace quantities of gold in real samples using ultrsound-assisted emulsification of solidified floating organic drops. Microchim Acta 173:249–257

    Article  Google Scholar 

  25. Ma JJ, Zhang JW, Du X, Lei X, Li JC (2010) Solidified floating organic drop microextraction for determination of trace amounts of zinc in water samples by flame atomic absorption spectrometry. Microchim Acta 168:153–159

    Article  CAS  Google Scholar 

  26. Chang QY, Feng T, Song SJ, Zhou X, Wang C, Wang Z (2010) Analysis of eight pyrethroids in water samples by liquid–liquid microextraction based on solidification of floating organic droplet combined with gas chromatography. Microchim Acta 171:241–247

    Article  CAS  Google Scholar 

  27. Xu H, Ding Z, Lv L, Song D, Feng YQ (2009) A novel dispersive liquid-liquid microextraction based on solidification of floating organic droplet method for determination of polycyclic aromatic hydrocarbons in aqueous samples. Anal Chim Acta 636:28–33

    Article  CAS  Google Scholar 

  28. Leong MI, Huang SD (2008) Dispersive liquid–liquid microextraction method based on solidification of floating organic drop combined with gas chromatography with electron-capture or mass spectrometry detection. J Chromatogr A 1211:8–12

    Article  CAS  Google Scholar 

  29. Cheng J, Xiao J, Zhou Y (2011) Dispersive liquid-liquid microextraction based on solidification of floating organic droplet method for the determination of diethofencarb and pyrimethanil in aqueous samples. Microchim Acta 172:51–55

    Article  CAS  Google Scholar 

  30. Chang CC, Huang SD (2010) Determination of the steroid hormone levels in water samples by dispersive liquid-liquid microextraction with solidification of a floating organic drop followed by high-performance liquid chromatography. Anal Chim Acta 662:39–43

    Article  CAS  Google Scholar 

Download references

Acknowledgment

This work was supported by the National Natural Science Foundation of China (No. 21176262) and Key Laboratory of Resources Chemistry of Nonferrous Metals, Ministry of Education (Central South University).

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Xinyu Jiang.

Electronic supplementary material

Below is the link to the electronic supplementary material.

ESM 1

(DOC 112 kb)

Rights and permissions

Reprints and permissions

About this article

Cite this article

Hou, F., Deng, T. & Jiang, X. Dispersive liquid-liquid microextraction of phenolic compounds using solidified floating organic droplets, and their determination by HPLC. Microchim Acta 180, 341–346 (2013). https://doi.org/10.1007/s00604-012-0937-8

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00604-012-0937-8

Keywords

Navigation