Chromatographia

, Volume 75, Issue 13–14, pp 739–745 | Cite as

Liquid Chromatographic Determination of 1,3,5-Trinitroperhydro-1,3,5-triazine and 2,4,6-Trinitrotoluene in Human Plasma and Groundwater Samples Utilizing Microextraction in Packed Syringe

  • Pooja Bansal
  • Gaurav
  • Nidhi
  • Ashok Kumar Malik
  • Frank-Michael Matysik
Original

Abstract

A rapid and efficient analytical method suitable for the simultaneous determination of 1,3,5-trinitroperhydro-1,3,5-triazine (RDX) and 2,4,6-trinitrotoluene (TNT) in groundwater and human plasma samples using liquid chromatography with UV detection (LC-UV) has been developed. RDX and TNT were baseline separated within time span of 4.8 min on a reverse phase C18 analytical column with water acetonitrile mixture in ratio 30:70 (v/v) as mobile phase. The UV detection was carried out at 234 nm. A sample preparation method for biological and environmental matrices using microextraction by packed sorbent (MEPS) technique has been implemented, employing 4 mg of C18 silica sorbent inserted into a microvolume syringe and using only 30 μL of plasma and groundwater samples. Several factors affecting the performance of MEPS, such as number of extraction cycles, washing solvent volume, elution solvent volume and carryover etc., were optimized. Limits of detection were 0.0997 and 0.0628 ng mL−1 for RDX and TNT, respectively. The extraction yields were satisfactory for both analytes (>81.2 %) as well as the precision data, which were always in the low percentage of relative standard deviation values (<5.6 % , n = 6). The present method is miniaturized, fully automated, and robust which can be easily used for forensic studies of explosives in environmental and biological samples.

Keywords

HPLC RDX TNT Explosives Microextraction MEPS 

References

  1. 1.
    Yinon J, Zitrin S (1993) Modern methods and applications in analysis of explosives. Wiley, New YorkGoogle Scholar
  2. 2.
    Narayanan TV (1996) Modern technologies of bomb detection and disposal. RA Security System, New DelhiGoogle Scholar
  3. 3.
    Yinon J (1999) Toxicity and metabolism of explosives. CRC Press, Boca RatonGoogle Scholar
  4. 4.
    Holmgren E, Carlsson H, Goede P, Crescenzi C (2005) J Chromatogr A 1099:127–135CrossRefGoogle Scholar
  5. 5.
    Hewitt AD, Jenkins TF, Walsh ME, Walsh MR, Taylor S (2005) Chemosphere 61:888–894CrossRefGoogle Scholar
  6. 6.
    Marple RL, LaCourse WR, Marple RL, LaCourse WR (2005) Anal Chem 77:6709–6714CrossRefGoogle Scholar
  7. 7.
    Marple RL, LaCourse WR (2005) Talanta 66:581–590CrossRefGoogle Scholar
  8. 8.
    Sanchez C, Carlsson H, Colmsjo A, Crescenzi C, Batlle R (2003) Anal Chem 75:4639–4645CrossRefGoogle Scholar
  9. 9.
    Harvey SD, Clauss TRW (1996) J Chromatogr A 753:81–89CrossRefGoogle Scholar
  10. 10.
    Feltes J, Levsen K (1989) J High Resolut Chromatogr 12:613–619CrossRefGoogle Scholar
  11. 11.
    Pan X, Zhang B, Cox SB, Anderson TA, Cobb GP (2006) J Chromatogr A 1107:2–8CrossRefGoogle Scholar
  12. 12.
    Pan X, Tian K, Jones LE, Cobb GP (2006) Talanta 70:455–459CrossRefGoogle Scholar
  13. 13.
    MacCrehan WA, Bedner M (2006) Forensic Sci Int 163:119–124CrossRefGoogle Scholar
  14. 14.
    Shin KH, Lim Y, Ahn JH, Khil J, Cha CJ, Hur HG (2005) Chemosphere 61:30–39CrossRefGoogle Scholar
  15. 15.
    Dutta SK, Hollowella GP, Hashemb FM, Kuykendallc LD (2003) Soil Biol Biochem 35:667–675CrossRefGoogle Scholar
  16. 16.
    Bausinger T, Dehner U, Preuss J (2004) Chemosphere 57:821–829CrossRefGoogle Scholar
  17. 17.
    Paull B, Roux C, Dawson M, Doble P (2004) J Forensic Sci 49:1181–1186CrossRefGoogle Scholar
  18. 18.
    Halasz A, Groom C, Zhou E, Paquet L, Beaulieu C, Deschamps S, Corriveau A, Thiboutot S, Ampleman G, Dubois C, Hawari J (2002) J Chromatogr A 963:411–418CrossRefGoogle Scholar
  19. 19.
    Batlle R, Carlsson H, Holmgren E, Colmsjo A, Crescenzi C (2002) J Chromatogr A 963:73–82CrossRefGoogle Scholar
  20. 20.
    Astratov M, Preiss A, Levsen K, Wiinsch G (1997) Int J Mass Spectrom Ion Processes 167/168:481–502Google Scholar
  21. 21.
    Levsen K, Mussmann P, Berger-Preiss E, Preiss A, Volmer D, Wuensch G (1993) Acta Hydrochim Hydrobiol 21:153–166CrossRefGoogle Scholar
  22. 22.
    Furton KG, Wu LM, Almirall JR (2000) J Forensic Sci 45:857–864Google Scholar
  23. 23.
    Monteil-Rivera F, Beaulieu C, Deschamps S, Paquet L, Hawari J (2004) J Chromatogr A 1048:213–221Google Scholar
  24. 24.
    Wu L, Almirall JR, Furton KG (1999) J High Resol Chromatogr 22:279–282CrossRefGoogle Scholar
  25. 25.
    Wynne P, Hibbert R, DiFeo D, Dawes P (2008) Column 4:12–17Google Scholar
  26. 26.
    El-Beqqali A, Abdel-Rehim M (2007) J Sep Sci 30:2501–2505CrossRefGoogle Scholar
  27. 27.
    Moeder M, Schrader S, Winkler U, Rodil R (2010) J Chromatogr A 1217:2925–2932CrossRefGoogle Scholar
  28. 28.
    Said R, Hassan Z, Hassan M, Abdel-Rehim M (2008) J Liq Chromatogr Rel Technol 31:683–694CrossRefGoogle Scholar
  29. 29.
    Prieto A, Vallejo A, Zuloaga O, Paschke A, Sellergen B, Schillinger E, Schrader S, Möder M (2011) Anal Chim Acta 703:41–51CrossRefGoogle Scholar
  30. 30.
    Abdel-Rehim M, Hassan Z, Skansem P, Hassan M (2007) J Liq Chromatogr Rel Technol 30:3029–3041CrossRefGoogle Scholar
  31. 31.
    Prieto A, Schrader S, Bauer C, Moder M (2011) Anal Chim Acta 685:146–152CrossRefGoogle Scholar
  32. 32.
    Vita M, Skansen P, Hassan M, Abdel-Rehim M (2005) J Chromatogr B 817:303–307CrossRefGoogle Scholar
  33. 33.
    Vlckova H, Solichova D, Blaha M, Solich P, Novakova L (2011) J Pharm Biomed Anal 55:301–308CrossRefGoogle Scholar
  34. 34.
    Vlckova H, Rabatinova M, Miksova A, Kolouchova G, Micuda S, Solich P, Novakova L (2012) Talanta 90:22–29CrossRefGoogle Scholar
  35. 35.
    Jonsson S, Hagberg J, Van Bavel B (2008) J Agric Food Chem 56:4962–4967CrossRefGoogle Scholar
  36. 36.
    Moreno IED, da Fonseca BM, Barroso M, Costa S, Queiroz JA, Gallardo E (2012) J Pharm Biomed Anal 61:93–99CrossRefGoogle Scholar
  37. 37.
    Miyaguchi H, Iwata YT, Kanamori T, Tsujikawa K, Kuwayama K, Inoue H (2009) J Chromatogr A 1216:4063–4070CrossRefGoogle Scholar
  38. 38.
    2002/657/EC Implementing Council Directive 96/23/EC. http://www.eur-lex.europa.eu

Copyright information

© Springer-Verlag 2012

Authors and Affiliations

  • Pooja Bansal
    • 1
  • Gaurav
    • 1
  • Nidhi
    • 2
  • Ashok Kumar Malik
    • 1
  • Frank-Michael Matysik
    • 3
  1. 1.Department of ChemistryPunjabi UniversityPatialaIndia
  2. 2.Department of ChemistryZakir Husain Delhi CollegeNew DelhiIndia
  3. 3.Universität Regensburg Institut für Analytische Chemie, Chemo-und BiosensorikRegensburgGermany

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