2009•Chinese Journal of Health Laboratory TechnologyRequires access

Automated solid phase extractin and hydrophilic interaction liquid chromatography for determination of melamine in raw milk and dairy products

Xiuyao Zhang

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Abstract

Objective:A approach for the determination of melamine in raw milk and dairy products by hydrophilic interaction liquid chromatography using automated solid phase extractin is described.Methods:Trichloroacetic acid solution was used to precipitate proteins and to dissociate the target analyte from the sample matrix.The extracted solution was cleaned-up with Oasis MCX SPE column using an automated solid phase extractin system.The HPLC separation was carried out on a Atlantis Hilic Silica column(4.6 mm×150 mm,3 μm) with acetonitrile-20 mmol/L ammonium acetate(90:10,v/v) as mobile phase at flow rate of 1.00 ml/min,and detected at UV 210 nm,then quantified by external standard calibration.Results:The limit of quantification(s/n=10) for melamine was 0.2 mg/kg.The recoveries were 87%~96% with the relative standard deviation of 0.8%~3.4%(n=5).Conclusion:This method is accurate and precise to detect melamine in raw milk and dairy products.

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Objective:A approach for the determination of melamine in raw milk and dairy products by hydrophilic interaction liquid chromatography using automated solid phase extractin is described.Methods:Trichloroacetic acid solution was used to precipitate proteins and to dissociate the target analyte from the sample matrix.The extracted solution was cleaned-up with Oasis MCX SPE column using an automated solid phase extractin system.The HPLC separation was carried out on a Atlantis Hilic Silica column(4.6 mm×150 mm,3 μm) with acetonitrile-20 mmol/L ammonium acetate(90:10,v/v) as mobile phase at flow rate of 1.00 ml/min,and detected at UV 210 nm,then quantified by external standard calibration.Results:The limit of quantification(s/n=10) for melamine was 0.2 mg/kg.The recoveries were 87%~96% with the relative standard deviation of 0.8%~3.4%(n=5).Conclusion:This method is accurate and precise to detect melamine in raw milk and dairy products.

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Available abstract

Objective:A approach for the determination of melamine in raw milk and dairy products by hydrophilic interaction liquid chromatography using automated solid phase extractin is described.Methods:Trichloroacetic acid solution was used to precipitate proteins and to dissociate the target analyte from the sample matrix.The extracted solution was cleaned-up with Oasis MCX SPE column using an automated solid phase extractin system.The HPLC separation was carried out on a Atlantis Hilic Silica column(4.6 mm×150 mm,3 μm) with acetonitrile-20 mmol/L ammonium acetate(90:10,v/v) as mobile phase at flow rate of 1.00 ml/min,and detected at UV 210 nm,then quantified by external standard calibration.Results:The limit of quantification(s/n=10) for melamine was 0.2 mg/kg.The recoveries were 87%~96% with the relative standard deviation of 0.8%~3.4%(n=5).Conclusion:This method is accurate and precise to detect melamine in raw milk and dairy products.

Key concepts: Melamine, Chromatography, Chemistry, Hydrophilic interaction chromatography, Ammonium acetate, Analyte, Detection limit, Trichloroacetic acid

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