Rapid Determination of Melamine in Pork by Solid Phase Extraction and HPLC Method
MA Yi-hong
Abstract
MA Yi-hong
Abstract
[Objective] The aim was to study determining melamine content in pork by using HPLC method,and strengthening monitor of melamine in food and feed.[Method]The pork sample was extracted by solution of methyl cyanide mixed with aqueous(7∶ 3,V/V),and purified by OasisMCX solid phase extraction column,the content of melamine in pork was determined by HPLC.[Result] The optimum working conditions were determined: methyl cyanide-0.05 mol/L phosphate buffer(7∶ 3,V/V),flow rate 1.5 ml/min,column temperature 35 ℃,wavelength 235 nm,injection volume 20 μl.Under this condition,melamine has good linear relationship at 0.1-100.0 mg/L,the correlation relationship is 0.999 89,the detection limit is 0.5 mg/kg.In the range of adding sample 0.5-5.0 mg/kg,the recovery rate is 86.0%-108.0%,RSD is less than 7.4%.[Conclusion]The method is easy,rapid,sensitive and accurate for determining melamine in pork.
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[Objective] The aim was to study determining melamine content in pork by using HPLC method,and strengthening monitor of melamine in food and feed.[Method]The pork sample was extracted by solution of methyl cyanide mixed with aqueous(7∶ 3,V/V),and purified by OasisMCX solid phase extraction column,the content of melamine in pork was determined by HPLC.[Result] The optimum working conditions were determined: methyl cyanide-0.05 mol/L phosphate buffer(7∶ 3,V/V),flow rate 1.5 ml/min,column temperature 35 ℃,wavelength 235 nm,injection volume 20 μl.Under this condition,melamine has good linear relationship at 0.1-100.0 mg/L,the correlation relationship is 0.999 89,the detection limit is 0.5 mg/kg.In the range of adding sample 0.5-5.0 mg/kg,the recovery rate is 86.0%-108.0%,RSD is less than 7.4%.[Conclusion]The method is easy,rapid,sensitive and accurate for determining melamine in pork.
Key concepts: Melamine, Chromatography, Cyanide, High-performance liquid chromatography, Chemistry, Extraction (chemistry), Detection limit, Solid phase extraction