2006Chinese Journal of ChromatographyRequires access

Determination of Multiple Pesticide Residues in Honey Using Gas Chromatography-Electron Impact Ionization-Mass Spectrometry

Zhitong Jin, Zhen Lin, Mingli Chen, Yan Ma, Jun Jie Tan, Yiqun Fan, Jin Wen, Zuliang Chen, Fengqin Tu

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Abstract

An analytical method was developed for the simultaneous determination of 23 pesticide residues in various commercial honeys. Meanwhile, the characteristic ions and fragmentation mechanism of three pesticides in the process of electron ionization mass spectrometry (EI/MS) were evaluated. After the optimization of different parameters such as the extraction solvent, pesticides were extracted from honey with ethyl acetate in an ultrasonic bath, cleaned up on a Florisil column by an elution of mixture of hexane and ethyl acetate (7:3, v/v), and analyzed by gas chromatography-electron ionization mass spectrometry (GC-EI/MS) in the selected ion monitoring mode (SIM) with PCB103 as internal standard. Recovery studies were performed at 50, 100 and 200 microg/kg fortification levels for each pesticide, and the recoveries ranged from 82% to 120% with relative st0ndard deviations between 1.8% and 11.0% for different pesticides. The limit of detection was less than 10.0 microg/kg for all the pesticides. The developed method was linear in the range of 10-500 microg/kg, with correlation coefficients larger than 0.995. Finally, the developed analytical method has been successfully applied to the determination of pesticide residues in several honey samples.

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What this paper is about

An analytical method was developed for the simultaneous determination of 23 pesticide residues in various commercial honeys. Meanwhile, the characteristic ions and fragmentation mechanism of three pesticides in the process of electron ionization mass spectrometry (EI/MS) were evaluated. After the optimization of different parameters such as the extraction solvent, pesticides were extracted from honey with ethyl acetate in an ultrasonic bath, cleaned up on a Florisil column by an elution of mixture of hexane and ethyl acetate (7:3, v/v), and analyzed by gas chromatography-electron ionization mass spectrometry (GC-EI/MS) in the selected ion monitoring mode (SIM) with PCB103 as internal standard. Recovery studies were performed at 50, 100 and 200 microg/kg fortification levels for each pesticide, and the recoveries ranged from 82% to 120% with relative st0ndard deviations between 1.8% and 11.0% for different pesticides. The limit of detection was less than 10.0 microg/kg for all the pesticides. The developed method was linear in the range of 10-500 microg/kg, with correlation coefficients larger than 0.995. Finally, the developed analytical method has been successfully applied to the determination of pesticide residues in several honey samples.

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Available abstract

An analytical method was developed for the simultaneous determination of 23 pesticide residues in various commercial honeys. Meanwhile, the characteristic ions and fragmentation mechanism of three pesticides in the process of electron ionization mass spectrometry (EI/MS) were evaluated. After the optimization of different parameters such as the extraction solvent, pesticides were extracted from honey with ethyl acetate in an ultrasonic bath, cleaned up on a Florisil column by an elution of mixture of hexane and ethyl acetate (7:3, v/v), and analyzed by gas chromatography-electron ionization mass spectrometry (GC-EI/MS) in the selected ion monitoring mode (SIM) with PCB103 as internal standard. Recovery studies were performed at 50, 100 and 200 microg/kg fortification levels for each pesticide, and the recoveries ranged from 82% to 120% with relative st0ndard deviations between 1.8% and 11.0% for different pesticides. The limit of detection was less than 10.0 microg/kg for all the pesticides. The developed method was linear in the range of 10-500 microg/kg, with correlation coefficients larger than 0.995. Finally, the developed analytical method has been successfully applied to the determination of pesticide residues in several honey samples.

Key concepts: Chemistry, Electron ionization, Chromatography, Mass spectrometry, Detection limit, Ethyl acetate, Pesticide residue, Chemical ionization

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