2009Journal of Zhejiang Ocean UniversityRequires access

High-performance Liquid Chromatography-tandem Mass Spectrometry for the Determination of the 21 Sulfonamide Residues in Eriocheir sinensis

Fan Zhou

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Abstract

The method of simultaneous determination of twenty commonly used sulfonamide residues in Eriocheir sinensis by high performance liquid chromatography-electro spray tandem mass spectrometry(HPLC/ MS/MS) is described.Sulfonamide residues were extracted from homogenized tissue with acetonitrile and dichloromethane.A part of the extract was taken and then dried by nitrogen.The residues were dissolved into 1 mL mobile phase and defatted with n-hexane(saturated by acetonitrile).The 21 analytes were separated on ZORBAX Eclipse XDB-C8 Column with mobile phases containingmethanol and 0.2% acetic acid and finally determined by electrospray ionization tandem mass spectrometry(ESI-MS-MS).A linear gradient eluting pro-gram of methanol from 30% to 80%(V/V) was employed at a flow rate of 0.2 mL/min in 35 minutes.Analytes confirmation were performed using multiple reaction monitoring(MRM) with one precursorion and two product ions as identifiers.The quantitative limit of method was 5 μg/kg.Recoveries tested by standard addition method were in the range of 71.8%-106%,RSDs were in the range of 0.44%-10.1% at a spiking level from 4 μg/kg to 40 μg/kg(n= 6).

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The method of simultaneous determination of twenty commonly used sulfonamide residues in Eriocheir sinensis by high performance liquid chromatography-electro spray tandem mass spectrometry(HPLC/ MS/MS) is described.Sulfonamide residues were extracted from homogenized tissue with acetonitrile and dichloromethane.A part of the extract was taken and then dried by nitrogen.The residues were dissolved into 1 mL mobile phase and defatted with n-hexane(saturated by acetonitrile).The 21 analytes were separated on ZORBAX Eclipse XDB-C8 Column with mobile phases containingmethanol and 0.2% acetic acid and finally determined by electrospray ionization tandem mass spectrometry(ESI-MS-MS).A linear gradient eluting pro-gram of methanol from 30% to 80%(V/V) was employed at a flow rate of 0.2 mL/min in 35 minutes.Analytes confirmation were performed using multiple reaction monitoring(MRM) with one precursorion and two product ions as identifiers.The quantitative limit of method was 5 μg/kg.Recoveries tested by standard addition method were in the range of 71.8%-106%,RSDs were in the range of 0.44%-10.1% at a spiking level from 4 μg/kg to 40 μg/kg(n= 6).

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Available abstract

The method of simultaneous determination of twenty commonly used sulfonamide residues in Eriocheir sinensis by high performance liquid chromatography-electro spray tandem mass spectrometry(HPLC/ MS/MS) is described.Sulfonamide residues were extracted from homogenized tissue with acetonitrile and dichloromethane.A part of the extract was taken and then dried by nitrogen.The residues were dissolved into 1 mL mobile phase and defatted with n-hexane(saturated by acetonitrile).The 21 analytes were separated on ZORBAX Eclipse XDB-C8 Column with mobile phases containingmethanol and 0.2% acetic acid and finally determined by electrospray ionization tandem mass spectrometry(ESI-MS-MS).A linear gradient eluting pro-gram of methanol from 30% to 80%(V/V) was employed at a flow rate of 0.2 mL/min in 35 minutes.Analytes confirmation were performed using multiple reaction monitoring(MRM) with one precursorion and two product ions as identifiers.The quantitative limit of method was 5 μg/kg.Recoveries tested by standard addition method were in the range of 71.8%-106%,RSDs were in the range of 0.44%-10.1% at a spiking level from 4 μg/kg to 40 μg/kg(n= 6).

Key concepts: Chemistry, Chromatography, Tandem mass spectrometry, Selected reaction monitoring, Mass spectrometry, Liquid chromatography–mass spectrometry, Electrospray ionization, Detection limit

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High-performance Liquid Chromatography-tandem Mass Spectrometry for the Determination of the 21 Sulfonamide Residues in Eriocheir sinensis — Research Paper | ScholarLens