Skip to main content
Log in

Dispersive solid-phase extraction for in-sorbent Fourier-transform infrared detection and identification of nerve agent simulants in analysis for verification of chemical weapon convention

  • Original Paper
  • Published:
Analytical and Bioanalytical Chemistry Aims and scope Submit manuscript

Abstract

The combination of dispersive solid-phase extraction (DSPE) and Fourier-transform infrared (FTIR) spectroscopy is presented for detection and quantification of markers and simulants of nerve agents. Hydrophilic–lipophilic balance (HLB) sorbent was used for extraction and enrichment of organophosphonates from water. When the extraction efficiency of DSPE was compared with that of conventional solid-phase extraction (SPE), DSPE was more efficient. Extraction conditions such as extraction time, and type and quantity of sorbent material were optimized. In DSPE, extracted analytes are detected and quantified on the sorbent using FTIR as analytical technique. Absorbance in FTIR due to P–O–C stretching was used for detection and quantification. Infrared absorbance of different analytes were compared by determining their molar absorptivities (ε max). Quantitative analyses were performed employing modified Beer’s law, and relative standard deviations (RSDs) for intraday repeatability and interday reproducibility were found to be in the range 0.30–0.90% and 0.10–0.80% respectively. The limit of detection (LOD) was 5–10 μg mL−1. The applicability of the method was tested with an unknown sample prepared by mimicking the sample obtained in an international official proficiency test.

Dispersive solid-phase extraction of nerve agents simulants coupled with Fourier transform infrared detection

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

  1. Messilakso M (2005) In: Messilakso M (ed) Chemical weapons convention chemical analysis sample collection, preparation and analytical methods. Chichester, Wiley

    Chapter  Google Scholar 

  2. Kientz CE (1998) J Chromatogr A 814:1–2

    Article  CAS  Google Scholar 

  3. Kostiainen O (2000) In: Bogusz MJ (ed) Handbook of analytical separations, vol. 2, forensic science. Elsevier, Amsterdam, p 405

    Google Scholar 

  4. Palit M, Pardasani D, Gupta AK, Dubey DK (2005) Anal Chem 77:711–717

    Article  CAS  Google Scholar 

  5. Dubey DK, Pardasani D, Palit M, Gupta AK, Jain R (2005) J Chromatogr A 1076:27–33

    Article  CAS  Google Scholar 

  6. Krutzch W, Trapp R (1994) A commentary of CWC. Martinus Nijhoff, The Netherlands

    Google Scholar 

  7. Convention on the Prohibition of the Development, Production, Stockpiling and Use of Chemical Weapons and their Destruction, Technical Secretariat of the Organization for Prohibition of Chemical Weapons (1997) The Hague. http://www.opcw.nl. Accessed 26 July 2010

  8. Messilakso M, Niederhauser A (2005) In: Messilakso M (ed) Chemical weapons convention chemical analysis. Wiley, Chichester, p 321

    Google Scholar 

  9. Hooijschuur EWJ, Kientz CE, Brinkman UAT (2002) J Chromatogr A 982:177–200

    Article  CAS  Google Scholar 

  10. Ragunathan N, Krock KA, Klawun C, Sasaki TA, Wilkins CL (1999) J Chromatogr A 856:349–397

    Article  CAS  Google Scholar 

  11. Mazumder A, Kumar A, Purohit AK, Dubey DK (2010) J Chromatogr A 1217:2887–2894

    Article  CAS  Google Scholar 

  12. Mazumder A, Gupta HK, Garg P, Jain R, Dubey DK (2009) J Chromatogr A 1216:5228–5234

    Article  CAS  Google Scholar 

  13. Tak V, Pardasani D, Kanaujia PK, Dubey DK (2009) J Chromatogr 1216:4319–4328

    Article  CAS  Google Scholar 

  14. Lendl B (2004) In: Analytical Chemistry, A Modern Approach to Analytical Science, Wiley, Weinheim, chap 25.2

  15. Veness RG, Evans CS (1996) J Chromatogr A 750:311–316

    Article  CAS  Google Scholar 

  16. Smith BC (1996) Ed. Fundamentals of Fourier-transform infrared spectroscopy. CRC, Boca Raton, FL

  17. Soderstrom MT, Ketola RA (1994) Fresenius J Anal Chem 350:162–167

    Article  Google Scholar 

  18. Soderstrom MT, Ketola RA, Kostiainen O (1995) Fresenius J Anal Chem 352:550–556

    Article  Google Scholar 

  19. Durst HD, Mayr JR, Ruth JL, Williams BR, Devil RA (1998) Anal Lett 31:1429–1444

    CAS  Google Scholar 

  20. Mcgarvey JJ, Stuff JR, Williams BR, Durst HD (2000) Spectrosc Lett 33:795–819

    Article  CAS  Google Scholar 

  21. Garg P, Purohit A, Tak VK, Dubey DK (2009) J Chromatogr A 1216:7906–7914

    Article  CAS  Google Scholar 

  22. Black RM, Muir B (2003) J Chromatogr A 1000:253–281

    Article  CAS  Google Scholar 

  23. Inon FA, Garrigues JM, Garrigues S, Molina A, Guardia M (2003) Anal Chim Acta 489:59–75

    Article  CAS  Google Scholar 

  24. Armenta S, Garrigues S, Guardia M (2007) Anal Chim Acta 596:330–337

    Article  CAS  Google Scholar 

  25. Setiowaty G, Man YBC, Jinap S, Moh MH (2000) Phytochem Anal 11:74–78

    Article  CAS  Google Scholar 

  26. Bertacche V, Pini E, Stradi R, Stratta F (2006) J Pharm Sci 95:159–166

    Article  CAS  Google Scholar 

  27. Kanaujia PK, Tak V, Pardasani D, Gupta AK, Dubey DK (2008) J Chromatogr A 1185:167–177

    Article  CAS  Google Scholar 

  28. Kanaujia PK, Pardasani D, Gupta AK, Kumar R, Srivastava RK, Dubey DK (2007) J Chromatogr A 1161:98–104

    Article  CAS  Google Scholar 

  29. Rautio M (1994) Recommended operating procedures for sampling and analysis in the verification of chemical disarmament. Ministry for Foreign Affairs of Finland, Helsinki

    Google Scholar 

  30. Kuitunen ML In: Mesilaakso M (2005) (ed.) Chemical Weapons Convention Chemical Analysis Sample Collection, Preparation and Analytical Methods. Wiley, Chichester, p 163

  31. Lakso HA (1997) Anal Chem 69:1866–1872

    Article  CAS  Google Scholar 

  32. Sng MT, Ng WF (1999) J Chromatogr A 832:173–182

    Article  CAS  Google Scholar 

  33. Dubey DK, Pardasani D, Gupta AK, Palit M, Kanaujia PK, Tak V (2006) J Chromatogr A 1107:29–35

    Article  CAS  Google Scholar 

  34. Lee HSN, Basheer C, Lee HK (2006) J Chromatogr A 1124:91–96

    Article  CAS  Google Scholar 

  35. Watson JM, Jhang GS, Payne PA (1992) J Membr Sci 73:55–71

    Article  CAS  Google Scholar 

  36. Karlowatz M, Kraft M, Mizaikoff B (2004) Anal Chem 76:2643–2648

    Article  CAS  Google Scholar 

  37. Burck J, Conzen JP, Ache AJ (1992) Fresenius J Anal Chem 342:394–400

    Article  Google Scholar 

  38. Flavin K, Mullowney J, Murphy B, Owens E, Kirwan P, Murphy K, Hughes H, McLoughlin P (2007) Analyst 132:224–229

    Article  CAS  Google Scholar 

  39. Regan F, Meaney M, Vos JG, MacCraith BD, Walsh JE (1996) Anal Chim Acta 334:85–92

    Article  CAS  Google Scholar 

  40. Lee MKV, Weg WGV, Traag WA, Mol HG (2008) J Chromatogr A 1186:325–339

    Article  Google Scholar 

  41. Leandr CC, Fussell RJ, Keely BJ (2005) J Chromatogr A 1085:207–212

    Article  Google Scholar 

  42. Paya P, Anastassiades M, Mack D, Sigalova I, Tasdelen B, Oliva J, Barba A (2007) Anal Bioanal Chem 389:1697–1714

    Article  CAS  Google Scholar 

  43. Ji F, Zhao LX, Yan W, Feng QZ, Lin JM (2008) J Sep Sci 31:961–968

    Article  CAS  Google Scholar 

  44. Krska R, Stubbings G, Crews R (2008) Anal Bioanal Chem 391:563–576

    Article  CAS  Google Scholar 

  45. Fagerquist CK, Lightfield AR, Lehotay S (2005) Anal Chem 77:1473–1482

    Article  CAS  Google Scholar 

  46. Kosolapoff GM (1950) Organophosphorus compounds Ch. 7. Wiley, New York

    Google Scholar 

  47. Kanaujia PK, Pardasani D, Gupta AK, Dubey DK (2007) J Chromatogr A 1139:185–190

    Article  CAS  Google Scholar 

  48. Liu Y, Czarnecki MA, Ozaki Y, Suzuki M, Iwahashi M (1995) Vibr Spectrosc 9:221–224

    Article  CAS  Google Scholar 

  49. Evaluation of Results, Eighteen Official OPCW Test (2006) Technical secretariat of organization for prohibition of chemical weapons. Hague, The Netherlands

    Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to D. K. Dubey.

Electronic supplementary materials

Below is the link to the electronic supplementary material.

Electronic Supplementary Material

(PDF 140 kb)

Rights and permissions

Reprints and permissions

About this article

Cite this article

Garg, P., Pardasani, D., Mazumder, A. et al. Dispersive solid-phase extraction for in-sorbent Fourier-transform infrared detection and identification of nerve agent simulants in analysis for verification of chemical weapon convention. Anal Bioanal Chem 399, 955–963 (2011). https://doi.org/10.1007/s00216-010-4337-9

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00216-010-4337-9

Keywords

Navigation