Determination of four β-agonist residues in creatural liver by gel permeation chromatography coupled with high performance liquid chromatography-tandem mass spectrometry
WU Shu-xiu
Abstract
WU Shu-xiu
Abstract
A method for the simultaneous analysis of clenbuterol,salbutamol,ractopamine and terbutalin residues in creatural liver was developed using high performance liquid chromatography—tandem mass spectrometry(LC-MS/MS) based on gel permeation chromatographic(GPC) purification.The homogenized samples were digested by β-glucuronidase enzyme,and extracted with ammonium acetate,further cleanup was performed on a MCX cartridge and a GCP,The selected ion monitoring(SIM) method was used for detection and quantified by the interal standard method.The calibration curves showed good linearities for clenbuterol in the range of 0.1 ~ 10 ng/mL and for ractopamine,salbutamol and terbutalin in the range of 1 ~ 100 ng/mL with correlation coefficients(r2) more than 0.999.The limits of detection of four β-agonists were in the ranges of 0.003 ~ 0.02 μg/kg.The limits of quantification were in the ranges of 0.009 ~ 0.06 μg/kg.The spiked recoveries ranged from 94.7% to106.1% with relative standard deviations less than 7.8%.This method was suitable for the identification and quantification of clenbuterol,ractopamine,salbutamol and terbutalin in creatural liver.
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A method for the simultaneous analysis of clenbuterol,salbutamol,ractopamine and terbutalin residues in creatural liver was developed using high performance liquid chromatography—tandem mass spectrometry(LC-MS/MS) based on gel permeation chromatographic(GPC) purification.The homogenized samples were digested by β-glucuronidase enzyme,and extracted with ammonium acetate,further cleanup was performed on a MCX cartridge and a GCP,The selected ion monitoring(SIM) method was used for detection and quantified by the interal standard method.The calibration curves showed good linearities for clenbuterol in the range of 0.1 ~ 10 ng/mL and for ractopamine,salbutamol and terbutalin in the range of 1 ~ 100 ng/mL with correlation coefficients(r2) more than 0.999.The limits of detection of four β-agonists were in the ranges of 0.003 ~ 0.02 μg/kg.The limits of quantification were in the ranges of 0.009 ~ 0.06 μg/kg.The spiked recoveries ranged from 94.7% to106.1% with relative standard deviations less than 7.8%.This method was suitable for the identification and quantification of clenbuterol,ractopamine,salbutamol and terbutalin in creatural liver.
Key concepts: Ractopamine, Chemistry, Chromatography, Clenbuterol, Detection limit, Mass spectrometry, Calibration curve, Tandem mass spectrometry