固相萃取与高效液相色谱法快速测定猪肉中的三聚氰胺

Rapid Determination of Melamine in Pork by Solid Phase Extraction and HPLC Method

[目的]研究高效液相色谱法测定猪肉中三聚氰胺含量的方法,加强食品和饲料中三聚氰胺的监控。[方法]猪肉样品经乙腈-水(7∶3,V/V)溶液提取,于OasisMCX固相萃取柱净化,采用高效液相色谱法测定猪肉中三聚氰胺的含量。[结果]确定仪器最佳工作条件为:流动相为乙腈-0.05 mol/L磷酸盐缓冲液(7∶3,V/V),流速为1.5 ml/min,柱温35℃,波长235 nm,进样量20μl。在此条件下,三聚氰胺在0.1～100.0 mg/L具有良好的线性关系,相关系数达0.999 89,对猪肉中三聚氰胺的检出限为0.5 mg/kg,在加标0.5～5.0mg/kg浓度范围内,回收率在86.0%～108.0%,相对标准偏差(RSD)小于7.4%。[结论]该方法操作简便、快速、灵敏、准确,适合于测定猪肉中的三聚氰胺。

[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.