Asian Journal of Research in Chemistry

Open Access Open Access  Restricted Access Subscription Access
Open Access Open Access Open Access  Restricted Access Restricted Access Subscription Access

Separation evaluation of selected organophosphorus fungicides by NP-TLC and RP-HPTLC


Affiliations
1 Regional Forensic Science Laboratory, Davanagere, India
2 Regional Forensic Science Laboratory, Gulbarga, India
3 Department of Studies in Biochemistry, Mysore University, Mysore, India
4 Forensic Science Laboratory, Bangalore, India
     

   Subscribe/Renew Journal


Poisoning by organophosphorus fungicides (OPFs) is although uncommon; recently, a few cases of deaths owing to the ingestion of OPFs were reported. Literatures on chromatographic separation of these fungicides are minimal. The evaluation of the efficacies of separation is of primary interest when it is contemplated from a forensic matrix. Hence, a study was undertaken to evaluate the efficacies of separation of three OPFs, namely ditalimfos D, edifenfos E, and tolclofos-methyl TM by NP-TLC on silica gel 60F254 and RP- HPTLC on silica gel 60RP-18 WF254. The relationship between the mobile phase composition (n-hexane-acetone for NP-TLC, and methanol-water for RPHPTLC) and RF values affirmed that with the increase in the acetone content in case of NP-TLC and decrease of the water content in RP-HPTLC resulted in the increase in RF values for the three OPFs. The three OPFs are completely separated from each other with RF0.04, except for the pair of compounds E-D in NP-TLC with mobile phase composition 10:0, and for the pair of compounds E-TM in case of RP-HPTLC with mobile phase compositions of 10:0, 7:3, 6.5:3.5 and 6:4. Under the chromatographic conditions used, D and TM were found to have higher RM values in normal phase and reverse phase, respectively. Ditalimfos was therefore adsorbed strongly in NP-TLC and tolclofosmethyl in RP-HPTLC. The peak resolution (RS) values in NP-TLC were greater than 1.5 for the pair of compounds ED, TM-E, and TM-D in solvent composition ratio of 9:1, 8.5:1.5, 8:2, and 7.5:2.5. RS values in RP-HPTLC were also higher for all the pair compounds, except for E-TM. The study revealed that the system of NP-TLC with mobile phase n-hexane-acetone (9:1) provided the optimum conditions for the separation of D, E, and TM as compared to RPHPTLC system. Complete separation of E from TM was not achieved in RP-HPTLC.

Keywords

NP-TLC, RP-HPTLC, Mobile Phase Composition, Peak Resolution
Subscription Login to verify subscription
User
Notifications
Font Size


  • De Waard MA. Mechanisms of action of the organophosphorus fungicide pyrazophos, WAU dissertation No. 596. 18 Oct 1974.

  • Tomlin CDS. The pesticide Manual: a world compendium, 11th edn., The British Crop Protection Council, Farnham, Surrey. 1997. pp. 238.

  • Poul JM. Biochemical changes in liver and plasma of rats after oral administration of edifenphos. Toxicol Lett. 16; 1983: 31-34.

  • Hartley D and Kidd H. Agrochemicals handbook, Royal Chemical Society, Nottingham. 1983. pp. A168.

  • Yasuhiko UJ. Fungal choline biosynthesis- a target for controlling rice blast. Pesticide Outlook. 12; 2001: 26-27.

  • http://sitem.herts.ac.uk/aeru/iupac/Reports (Ref: DOWCO 199)

  • Thyssen J, Kimmerle G and Hinosan. 50 E.C./Toxicological Studies, Unpublished report from Institut für Toxikologie, Bayer A.G., submitted to the WHO by Bayer A.G. 1974.

  • Worthing CR and Hance RJ. The pesticide manual: a world compendium, 9th edn., The British Crop Protection Council, Farnham, Surrey. 1991.

  • Obana H, Kikuchi K, Okihashi M and Hori S. Determination of organophosphorus pesticides in foods using an accelerated solvent extraction system. Analyst. 122; 1997: 217-220.

  • Sasaki K, Suzuki T and Saito Y. Simplified cleanup and gas chromatographic determination of organophosphorus pesticides in crops. J AOAC. 70; 1987: 460-464.

  • Yukiko O, Takashi Y, Takeshi N and Toshiaki T. Pesticide multiresidue analysis of 303 compounds using supercritical fluid extraction. J Analytical Sciences. 22; 2006: 1473-1476.

  • Musshoff F, Junker H and Madea B. Simple determination of 22 organophosphorus pesticides in human blood using headspace solid-phase microextraction and gas chromatography with mass spectrometric detection. J Chromatogr Sci. 40; 2002: 29-34.

  • Blasco C, Font G and Pico Y. Solid-phase microextraction-liquid chromatography/tandem mass spectrometry to determine postharvest fungicides in fruits. Anal Chem. 75; 2003: 3606- 3615.

  • Blasco C, Pico Y, Manes J and Font G. Determination of fungicide residues in fruits and vegetables by liquid chromatography-atmospheric pressure chemical ionization mass spectrometry. J Chromatogr Sci. 947; 2002: 227-235.

  • Park KY, Park WC, Kim YJ and Lee YT. Development of an enzyme-linked immunosorbent assay for the organophosphorus fungicide tolclofos-methyl. Bull Korean Chem Soc. 24; 2003: 334-338.

  • Bazylak G, Brozik H and Sabanty W. Combined SPE and HPTLC as a screening assay of urinary cotinine from male adolescents exposed to environmental tobacco smoke. Polish Journal of Environmental Studies. 9; 2000: 113-123.

  • Sarbu C, Demertzis MA and Kovala – Demerrtzi D. Thin-layer chromatographic estimation of the lipophilicity of some metallic complexes of diclofenac with potential anti-inflammatory activity. Acta Chromatogr. 10; 2000: 222-229.

  • Acanski MM, Santa SJ and Jevric LR. Normal and reversed phase thin-layer chromatography of new 16, 17-secoestrone derivatives. J Serb Chem Soc. 68; 2003: 57-63.

  • Sherma J and Fried B. Handbook of Thin-layer Chromatography, edn. 3, CRC Press, Boca raton. 2003.

  • Lepri L, Cincinelli A and Del Bubba M. TLC of selected bile acids: detection and separation. J Planar Chromatogr- Mod TLC. 12; 1999: 298-301.

  • Miszczyk M and Pyka A. Comparision of normal and reversedphase TLC for separation of selected pesticide. J. Planar Chromatogr. 19; 2006: 15-20.

  • Pyka A and Klimczok W. Application of densitometry for the evaluation of the separation effect of nicotinic acid derivatives. Part I. Nicotinic acid and its amides. J Liq Chromatogr & Relat Technol. 30; 2007: 2317-2327.

  • Pyka A. TLC of selected bile acids: detection and separation. J Liq Chromatogr & Relat Technol. 31; 2008: 1373-1385.

  • Fried B and Sherma J. Thin-layer Chromatography, edn. 4, CRC Press, Boca raton. 1999.


Abstract Views: 345

PDF Views: 2




  • Separation evaluation of selected organophosphorus fungicides by NP-TLC and RP-HPTLC

Abstract Views: 345  |  PDF Views: 2

Authors

Purigali M Nagaraju
Regional Forensic Science Laboratory, Davanagere, India
Praveen U Sanganalmath
Regional Forensic Science Laboratory, Gulbarga, India
Kempaiah Kemparaju
Department of Studies in Biochemistry, Mysore University, Mysore, India
Bannur M Mohan
Forensic Science Laboratory, Bangalore, India

Abstract


Poisoning by organophosphorus fungicides (OPFs) is although uncommon; recently, a few cases of deaths owing to the ingestion of OPFs were reported. Literatures on chromatographic separation of these fungicides are minimal. The evaluation of the efficacies of separation is of primary interest when it is contemplated from a forensic matrix. Hence, a study was undertaken to evaluate the efficacies of separation of three OPFs, namely ditalimfos D, edifenfos E, and tolclofos-methyl TM by NP-TLC on silica gel 60F254 and RP- HPTLC on silica gel 60RP-18 WF254. The relationship between the mobile phase composition (n-hexane-acetone for NP-TLC, and methanol-water for RPHPTLC) and RF values affirmed that with the increase in the acetone content in case of NP-TLC and decrease of the water content in RP-HPTLC resulted in the increase in RF values for the three OPFs. The three OPFs are completely separated from each other with RF0.04, except for the pair of compounds E-D in NP-TLC with mobile phase composition 10:0, and for the pair of compounds E-TM in case of RP-HPTLC with mobile phase compositions of 10:0, 7:3, 6.5:3.5 and 6:4. Under the chromatographic conditions used, D and TM were found to have higher RM values in normal phase and reverse phase, respectively. Ditalimfos was therefore adsorbed strongly in NP-TLC and tolclofosmethyl in RP-HPTLC. The peak resolution (RS) values in NP-TLC were greater than 1.5 for the pair of compounds ED, TM-E, and TM-D in solvent composition ratio of 9:1, 8.5:1.5, 8:2, and 7.5:2.5. RS values in RP-HPTLC were also higher for all the pair compounds, except for E-TM. The study revealed that the system of NP-TLC with mobile phase n-hexane-acetone (9:1) provided the optimum conditions for the separation of D, E, and TM as compared to RPHPTLC system. Complete separation of E from TM was not achieved in RP-HPTLC.

Keywords


NP-TLC, RP-HPTLC, Mobile Phase Composition, Peak Resolution

References