气相色谱-质谱法测定粮油制品中的二甲基黄和二乙基黄含量

目的建立气相色谱-质谱法测定粮油制品中二甲基黄和二乙基黄的含量的分析方法。方法试样以1%醋酸的乙腈提取,采用油基质萃取管净化和HP-5MS色谱柱分离,质谱采用全扫描和选择离子模式测定,以外标法定量。同时考察了不同的提取溶剂及净化方式对回收率的影响。结果在添标水平为1、10和25 mg/kg时,二甲基黄和二乙基黄的平均回收率为76.3%~89.3%,相对标准偏差为3.0%~8.7%,二甲基黄的方法检出限为0.002 mg/kg,二乙基黄的检出限为0.001 mg/kg,符合检测方法参数的确认要求。结论该方法快速、准确,适用于粮油制品中的二甲基黄和二乙基黄含量。

Determination of dimethyl yellow and diethyl yellow in cereal and oilseeds products by gas chromatography-mass spectrometry

To establish a GC-MS method for determination of dimethyl yellow and methyl yellow in cereal and oilseeds products for the first time. The effects of ways of extraction and purification on the recovery have been studied. The samples were extracted by acetonitrile with dSPE purified column. HP-5 MS and MSD were used for determination. The average recoveries were in the range of 76%-89% at spiked levels of 1-25mg/kg,relative standard deviation of the methods were 4.8%-8.7%,and the limit of quantification of dimethyl yellow was 0.002mg/kg while that of methyl yellow was 0.001mg/kg, which both meet the requirement of technical parameters for analysis