Determination of residues of chloramphenicol in chicken muscle by matrix solid phase dispersion and ultra- performance liquid chromatography tandem mass spectrometry
Pan Xiao-don
Abstract
Pan Xiao-don
Abstract
Objective To develop a quantification method for chloramphenicol( CAP) in chicken muscle by matrix solid phase dispersion( MSPD) and ultra- performance liquid chromatography tandem mass spectrometry( UPLC- MS / MS). Methods Coupled with internal standard of d5- chloramphenicol,samples were extracted by matrix solid phase dispersion of C18 materials,and washed by hexane,then eluted with acetonitrile / water( V∶V,50∶50) The analyte in elution was then extracted by acetic ether,and dried by nitrogen extracted. The extraction was finally dissolved in mobile phase solvent. CAP was separated by gradient elution with methanol- water in ACQUITY BEH C18 column. The analyte was quantified by the isotope internal standard under the negative ion mode and multiple reactions monitoring mode. Results The limit of detection for CAP was 0. 01 μg / kg.The sample was spiking with CAP at level of 0. 5 μg / kg,10 μg / kg,and 50 μg / kg. The spiking average recoveries were85. 0% ~ 97. 3%,and the relative standard deviation varied between 5. 4% and 6. 8%. Conclusion The method was selective,sensitive,accurate and suitable for determination of trace CAP analysis in chicken muscle.
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Objective To develop a quantification method for chloramphenicol( CAP) in chicken muscle by matrix solid phase dispersion( MSPD) and ultra- performance liquid chromatography tandem mass spectrometry( UPLC- MS / MS). Methods Coupled with internal standard of d5- chloramphenicol,samples were extracted by matrix solid phase dispersion of C18 materials,and washed by hexane,then eluted with acetonitrile / water( V∶V,50∶50) The analyte in elution was then extracted by acetic ether,and dried by nitrogen extracted. The extraction was finally dissolved in mobile phase solvent. CAP was separated by gradient elution with methanol- water in ACQUITY BEH C18 column. The analyte was quantified by the isotope internal standard under the negative ion mode and multiple reactions monitoring mode. Results The limit of detection for CAP was 0. 01 μg / kg.The sample was spiking with CAP at level of 0. 5 μg / kg,10 μg / kg,and 50 μg / kg. The spiking average recoveries were85. 0% ~ 97. 3%,and the relative standard deviation varied between 5. 4% and 6. 8%. Conclusion The method was selective,sensitive,accurate and suitable for determination of trace CAP analysis in chicken muscle.
Key concepts: Chromatography, Chemistry, Elution, Solid phase extraction, Analyte, Detection limit, Mass spectrometry, Matrix (chemical analysis)