2007Chinese Journal of Veterinary DrugRequires access

Determination of Chloramphenicol Residue in the Eel by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

Li Yongfu

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Abstract

An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was developed to determine the residue of chloramphenicol in eel.The samples,labled by the isotopically internal standard,were finally dissolved in the mobile phase after the procedure of hydrolysis by 1% HCl,extraction by ethyl acetate,and purification.Chromatographic separation was achieved by using a Waters ACQUITY UPLCTM BEH C18 column and the detection was performed by tandem mass spectrometry under the mode of multiple reaction monitoring(MRM).The quantitative analysis of chloramphenicol was finished within 2 min.Results showed that in the range of 0.02~1.0 μg/kg the standard curves for chloramphenicol were in good linearity,and the correlation coefficients(r) was 0.996 5.The recoveries for chloramphenicol at the addition of three levels(0.05,0.1,0.5 μg/kg) were ranged from 86.6% to 92.5% and the relative standard deviation(RSD) for the determination of chloramphenicol was less than 8%(n = 5).The limit of quantity(LOQ) and limit of determination(LOD) by the present method for chloramphenicol were found to be 0.003 μg/kg and 0.011 μg/kg respectively.

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An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was developed to determine the residue of chloramphenicol in eel.The samples,labled by the isotopically internal standard,were finally dissolved in the mobile phase after the procedure of hydrolysis by 1% HCl,extraction by ethyl acetate,and purification.Chromatographic separation was achieved by using a Waters ACQUITY UPLCTM BEH C18 column and the detection was performed by tandem mass spectrometry under the mode of multiple reaction monitoring(MRM).The quantitative analysis of chloramphenicol was finished within 2 min.Results showed that in the range of 0.02~1.0 μg/kg the standard curves for chloramphenicol were in good linearity,and the correlation coefficients(r) was 0.996 5.The recoveries for chloramphenicol at the addition of three levels(0.05,0.1,0.5 μg/kg) were ranged from 86.6% to 92.5% and the relative standard deviation(RSD) for the determination of chloramphenicol was less than 8%(n = 5).The limit of quantity(LOQ) and limit of determination(LOD) by the present method for chloramphenicol were found to be 0.003 μg/kg and 0.011 μg/kg respectively.

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Available abstract

An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was developed to determine the residue of chloramphenicol in eel.The samples,labled by the isotopically internal standard,were finally dissolved in the mobile phase after the procedure of hydrolysis by 1% HCl,extraction by ethyl acetate,and purification.Chromatographic separation was achieved by using a Waters ACQUITY UPLCTM BEH C18 column and the detection was performed by tandem mass spectrometry under the mode of multiple reaction monitoring(MRM).The quantitative analysis of chloramphenicol was finished within 2 min.Results showed that in the range of 0.02~1.0 μg/kg the standard curves for chloramphenicol were in good linearity,and the correlation coefficients(r) was 0.996 5.The recoveries for chloramphenicol at the addition of three levels(0.05,0.1,0.5 μg/kg) were ranged from 86.6% to 92.5% and the relative standard deviation(RSD) for the determination of chloramphenicol was less than 8%(n = 5).The limit of quantity(LOQ) and limit of determination(LOD) by the present method for chloramphenicol were found to be 0.003 μg/kg and 0.011 μg/kg respectively.

Key concepts: Chromatography, Chemistry, Chloramphenicol, Detection limit, Residue (chemistry), Mass spectrometry, Selected reaction monitoring, Tandem mass spectrometry

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