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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。
Objective To establish a method for the determination of dimethyl yellow and diethyl yellow in grain and oil products by gas chromatography-mass spectrometry. Methods The samples were extracted with 1% acetic acid in acetonitrile, purified by oil matrix extraction and separated on a HP-5MS column. The mass spectra were determined by full scan and selected ion mode and quantified by external standard method. The effects of different extraction solvents and purification methods on recovery were also investigated. Results The average recoveries of dimethyl yellow and diethyl yellow were 76.3% ~ 89.3% with relative standard deviations of 3.0% ~ 8.7% at the levels of 1, 10 and 25 mg / kg. The dimethyl yellow The detection limit of the method was 0.002 mg / kg and the detection limit of diethyl yellow was 0.001 mg / kg, which met the confirmation requirements of the test method parameters. Conclusion The method is rapid and accurate and suitable for the determination of dimethyl yellow and diethyl yellow in grain and oil products.