论文部分内容阅读
研究建立了使用气相色谱串联质谱(GC/MS/MS)检测牛肉中三聚氰胺的分析方法。对牛肉中的三聚氰胺用0.1%三氯乙酸溶液和乙腈超声提取,经混合型阳离子交换固相萃取柱净化,净化液进行硅烷化衍生,衍生产物采用多反应监测(MRM)质谱扫描模式,用化合物的保留时间和质谱碎片的丰度比定性,外标法定量。在0.005 mg/L~1.0 mg/L范围内具有良好的线性关系,相关系数为0.999 8。方法最低定量限为0.005 mg/kg。牛肉中4种不同添加浓度0.05 mg/kg,0.10 mg/kg,0.50 mg/kg和1.0 mg/kg下三聚氰胺平均回收率范围为85%~110%,相对偏差小于10%。此方法样品前处理简单、定量限低、定性准确,适用于测定牛肉中的三聚氰胺。
A method was developed for the determination of melamine in beef using gas chromatography-tandem mass spectrometry (GC / MS / MS). The melamine in beef was extracted with 0.1% trichloroacetic acid solution and acetonitrile by ultrasonic extraction. The mixed solution was purified by mixed cation-exchange solid-phase extraction (SPE) column. The purified solution was silanized and the derivative was detected by MRM. The retention time and the abundance of MS fragments were qualitatively and quantitatively determined by external standard method. In the range of 0.005 mg / L to 1.0 mg / L, there was a good linear relationship with a correlation coefficient of 0.999 8. The minimum limit of quantitation was 0.005 mg / kg. The average recoveries of melamine at 0.05 mg / kg, 0.10 mg / kg, 0.50 mg / kg and 1.0 mg / kg in beef ranged from 85% to 110% and the relative deviation was less than 10%. This method is simple sample pretreatment, low quantitative limit, qualitative and accurate, suitable for the determination of melamine in beef.