2010Chinese Journal of Health Laboratory TechnologyRequires access

Simultaneous determination of twenty trace sulfonamides residues in honey by ultra-fast liquid chromatography coupled with tandem mass spectrometry

Xiaohong Chen

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Abstract

Objective:To develop a fast,efficient,accurate and sensitive method for determination of sulfonamides residues in honey by ultra-fast liquid chromatography tandem mass spectrometry.Methods: Honey samples were extracted using 0.1%(V/V) phosphoric acid,and purified by MCX solid-phase extraction(SPE) cartridges.The separation was carried out on a Shim-pack XR-ODS Ⅱ(100 mm×2.0 mm i.d.,2.2 μm) with acetonitrile and water as mobile phase by gradient elution,which containing 0.1%(V/V) formic acid and 5 mmol/L ammonium acetate.Detection was performed by an ultra-fast liquid chromatography-triple quadrupole tandem mass spectrometry(UFLC-MS/MS) with an electrospray ion(ESI) source in the positive multipile reaction monitoring(MRM) mode.Results: Calibration curves for the sulfonamides except sulfaguanidine and sulfacetamide were linear within the range of 0.25 μg/kg~25.0 μg/kg,and 1.0 μg/kg~25.0 μg/kg for sulfaguanidine and sulfacetamide.The correlation coefficients were more than 0.99,the limits of detection(LODs)were between 0.004 μg/kg~0.25 μg/kg,and the limits of quantification(LOQs)were between 0.01 μg/kg~0.83 μg/kg.The extraction recoveries ranged from 63.3% to 106.9% at three spiked levels of 0.5 μg/kg,2.5 μg/kg,5.0 μg/kg for each sulfonamide,and the RSDs ranged from 1.7% to 12.3%.Conclusion: The developed method can be detected simultaneously 20 sulfonamides within 5.5 min.It is fast and efficient,and which has used satisfactorily for the determination of trace sulfonamides in actual honey samples.

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Objective:To develop a fast,efficient,accurate and sensitive method for determination of sulfonamides residues in honey by ultra-fast liquid chromatography tandem mass spectrometry.Methods: Honey samples were extracted using 0.1%(V/V) phosphoric acid,and purified by MCX solid-phase extraction(SPE) cartridges.The separation was carried out on a Shim-pack XR-ODS Ⅱ(100 mm×2.0 mm i.d.,2.2 μm) with acetonitrile and water as mobile phase by gradient elution,which containing 0.1%(V/V) formic acid and 5 mmol/L ammonium acetate.Detection was performed by an ultra-fast liquid chromatography-triple quadrupole tandem mass spectrometry(UFLC-MS/MS) with an electrospray ion(ESI) source in the positive multipile reaction monitoring(MRM) mode.Results: Calibration curves for the sulfonamides except sulfaguanidine and sulfacetamide were linear within the range of 0.25 μg/kg~25.0 μg/kg,and 1.0 μg/kg~25.0 μg/kg for sulfaguanidine and sulfacetamide.The correlation coefficients were more than 0.99,the limits of detection(LODs)were between 0.004 μg/kg~0.25 μg/kg,and the limits of quantification(LOQs)were between 0.01 μg/kg~0.83 μg/kg.The extraction recoveries ranged from 63.3% to 106.9% at three spiked levels of 0.5 μg/kg,2.5 μg/kg,5.0 μg/kg for each sulfonamide,and the RSDs ranged from 1.7% to 12.3%.Conclusion: The developed method can be detected simultaneously 20 sulfonamides within 5.5 min.It is fast and efficient,and which has used satisfactorily for the determination of trace sulfonamides in actual honey samples.

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Available abstract

Objective:To develop a fast,efficient,accurate and sensitive method for determination of sulfonamides residues in honey by ultra-fast liquid chromatography tandem mass spectrometry.Methods: Honey samples were extracted using 0.1%(V/V) phosphoric acid,and purified by MCX solid-phase extraction(SPE) cartridges.The separation was carried out on a Shim-pack XR-ODS Ⅱ(100 mm×2.0 mm i.d.,2.2 μm) with acetonitrile and water as mobile phase by gradient elution,which containing 0.1%(V/V) formic acid and 5 mmol/L ammonium acetate.Detection was performed by an ultra-fast liquid chromatography-triple quadrupole tandem mass spectrometry(UFLC-MS/MS) with an electrospray ion(ESI) source in the positive multipile reaction monitoring(MRM) mode.Results: Calibration curves for the sulfonamides except sulfaguanidine and sulfacetamide were linear within the range of 0.25 μg/kg~25.0 μg/kg,and 1.0 μg/kg~25.0 μg/kg for sulfaguanidine and sulfacetamide.The correlation coefficients were more than 0.99,the limits of detection(LODs)were between 0.004 μg/kg~0.25 μg/kg,and the limits of quantification(LOQs)were between 0.01 μg/kg~0.83 μg/kg.The extraction recoveries ranged from 63.3% to 106.9% at three spiked levels of 0.5 μg/kg,2.5 μg/kg,5.0 μg/kg for each sulfonamide,and the RSDs ranged from 1.7% to 12.3%.Conclusion: The developed method can be detected simultaneously 20 sulfonamides within 5.5 min.It is fast and efficient,and which has used satisfactorily for the determination of trace sulfonamides in actual honey samples.

Key concepts: Chemistry, Chromatography, Formic acid, Selected reaction monitoring, Mass spectrometry, Detection limit, Extraction (chemistry), Tandem mass spectrometry

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