2011Chinese Journal of Analysis LaboratoryRequires access

Simultaneous determination of 24 sulfonamides residues in animal products by high performance liquid chromatography tandem mass spectrometry

She Yongxin

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Abstract

A selective and sensitive method has been developed and applied to the simultaneous determination of residue levels of sulfonamides in chicken,pork,beef,mutton,honey and bovine milk samples in 28 minutes using liquid chromatography tandem mass spectrometric(LC-MS/MS).The sulfonamides were extracted with acetonitrile,followed by homogenizing,ultrasound treating and centrifuging.The extract was dried by rotary evaporator,redissolved in the initial mobile phase and defatted with n-hexane saturated by acetonitrile(except the honey).The chromatographic analysis was performed on a Agilent Eclipse XDB-C18 column(2.1×150 mm,5 μm)using a gradient elution program of 0.2% acetic acid and acetonitrile as a mobile phase.The flow rate is 0.2 mL/min.Using LC-MS/MS(ESI) with multiple reaction monitoring(MRM),identification of the major components of 24 sulfonamides were performed based upon the intensities of mass fragments.Recoveries of 24 sulfonamides at the spiked concentration levels of 10 μg/kg,20μg/kg and 50μg/kg ranged from 60.8% to 122.9% with RSD,were 0.01%~19%,The calibration curves showed good linearity in the range of 5~300 μg/L for all sulfonamides with detection limits of 0.27~7.45 μg/kg and quantization limits of 0.957~9.89 μg/kg.The testing results of different laboratories have no significant differences.The method is suitable for quantitative and qualitative analysis of sulfonamides in a variety of samples.

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A selective and sensitive method has been developed and applied to the simultaneous determination of residue levels of sulfonamides in chicken,pork,beef,mutton,honey and bovine milk samples in 28 minutes using liquid chromatography tandem mass spectrometric(LC-MS/MS).The sulfonamides were extracted with acetonitrile,followed by homogenizing,ultrasound treating and centrifuging.The extract was dried by rotary evaporator,redissolved in the initial mobile phase and defatted with n-hexane saturated by acetonitrile(except the honey).The chromatographic analysis was performed on a Agilent Eclipse XDB-C18 column(2.1×150 mm,5 μm)using a gradient elution program of 0.2% acetic acid and acetonitrile as a mobile phase.The flow rate is 0.2 mL/min.Using LC-MS/MS(ESI) with multiple reaction monitoring(MRM),identification of the major components of 24 sulfonamides were performed based upon the intensities of mass fragments.Recoveries of 24 sulfonamides at the spiked concentration levels of 10 μg/kg,20μg/kg and 50μg/kg ranged from 60.8% to 122.9% with RSD,were 0.01%~19%,The calibration curves showed good linearity in the range of 5~300 μg/L for all sulfonamides with detection limits of 0.27~7.45 μg/kg and quantization limits of 0.957~9.89 μg/kg.The testing results of different laboratories have no significant differences.The method is suitable for quantitative and qualitative analysis of sulfonamides in a variety of samples.

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Available abstract

A selective and sensitive method has been developed and applied to the simultaneous determination of residue levels of sulfonamides in chicken,pork,beef,mutton,honey and bovine milk samples in 28 minutes using liquid chromatography tandem mass spectrometric(LC-MS/MS).The sulfonamides were extracted with acetonitrile,followed by homogenizing,ultrasound treating and centrifuging.The extract was dried by rotary evaporator,redissolved in the initial mobile phase and defatted with n-hexane saturated by acetonitrile(except the honey).The chromatographic analysis was performed on a Agilent Eclipse XDB-C18 column(2.1×150 mm,5 μm)using a gradient elution program of 0.2% acetic acid and acetonitrile as a mobile phase.The flow rate is 0.2 mL/min.Using LC-MS/MS(ESI) with multiple reaction monitoring(MRM),identification of the major components of 24 sulfonamides were performed based upon the intensities of mass fragments.Recoveries of 24 sulfonamides at the spiked concentration levels of 10 μg/kg,20μg/kg and 50μg/kg ranged from 60.8% to 122.9% with RSD,were 0.01%~19%,The calibration curves showed good linearity in the range of 5~300 μg/L for all sulfonamides with detection limits of 0.27~7.45 μg/kg and quantization limits of 0.957~9.89 μg/kg.The testing results of different laboratories have no significant differences.The method is suitable for quantitative and qualitative analysis of sulfonamides in a variety of samples.

Key concepts: Chemistry, Chromatography, Acetonitrile, Residue (chemistry), Calibration curve, Mass spectrometry, Liquid chromatography–mass spectrometry, Acetic acid

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