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GC Determination of Residual Amounts of Organophosphorus Pesticides in Tobacco

Zhao Ji-shou

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Abstract

Five organophosphorus pesticides as residues remained in tobacco were determined by gas chromatography with pulse flame photometric detector(PFPD).The powdered tobacco sample,after dehydration,was extracted with acetonitrile ultrasonically for 1 h,and the extract was evaporated to near dryness with a rotary evaporator.The residue was taken up with ethyl acetate,cyclohexane and a mixture of NaCl and anhydrous Na2SO4(mixed in the ratio of 1 to 1 by mass).The supernatant was taken and purified by gel permeation chromatography with a mixture of cyclohexane and ethyl acetate(mixed in the ratio of 1 to 1 by vol.) as mobile phase for elution.The eluate was collected,concentrated to 1 mL and diluted to 5.0 mL with ethyl acetate.One μL of the solution was taken for GC analysis.HP-5 elastic quartz capillary column was used for separation,and method of external standard was adopted in the determination.Detection limits(3S/N) for the 5 pesticides were in the range from 0.02 to 0.04 mg·L-1.Recovery and precision were tested and results of recovery obtained were in the range of 81.4% to 99.8%,with values of RSD′s(n=6) ranged from 3.27% to 8.42%.

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Five organophosphorus pesticides as residues remained in tobacco were determined by gas chromatography with pulse flame photometric detector(PFPD).The powdered tobacco sample,after dehydration,was extracted with acetonitrile ultrasonically for 1 h,and the extract was evaporated to near dryness with a rotary evaporator.The residue was taken up with ethyl acetate,cyclohexane and a mixture of NaCl and anhydrous Na2SO4(mixed in the ratio of 1 to 1 by mass).The supernatant was taken and purified by gel permeation chromatography with a mixture of cyclohexane and ethyl acetate(mixed in the ratio of 1 to 1 by vol.) as mobile phase for elution.The eluate was collected,concentrated to 1 mL and diluted to 5.0 mL with ethyl acetate.One μL of the solution was taken for GC analysis.HP-5 elastic quartz capillary column was used for separation,and method of external standard was adopted in the determination.Detection limits(3S/N) for the 5 pesticides were in the range from 0.02 to 0.04 mg·L-1.Recovery and precision were tested and results of recovery obtained were in the range of 81.4% to 99.8%,with values of RSD′s(n=6) ranged from 3.27% to 8.42%.

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Available abstract

Five organophosphorus pesticides as residues remained in tobacco were determined by gas chromatography with pulse flame photometric detector(PFPD).The powdered tobacco sample,after dehydration,was extracted with acetonitrile ultrasonically for 1 h,and the extract was evaporated to near dryness with a rotary evaporator.The residue was taken up with ethyl acetate,cyclohexane and a mixture of NaCl and anhydrous Na2SO4(mixed in the ratio of 1 to 1 by mass).The supernatant was taken and purified by gel permeation chromatography with a mixture of cyclohexane and ethyl acetate(mixed in the ratio of 1 to 1 by vol.) as mobile phase for elution.The eluate was collected,concentrated to 1 mL and diluted to 5.0 mL with ethyl acetate.One μL of the solution was taken for GC analysis.HP-5 elastic quartz capillary column was used for separation,and method of external standard was adopted in the determination.Detection limits(3S/N) for the 5 pesticides were in the range from 0.02 to 0.04 mg·L-1.Recovery and precision were tested and results of recovery obtained were in the range of 81.4% to 99.8%,with values of RSD′s(n=6) ranged from 3.27% to 8.42%.

Key concepts: Chromatography, Chemistry, Ethyl acetate, Elution, Gas chromatography, Anhydrous, Cyclohexane, Flame ionization detector

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