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

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

中文关键词:  气相色谱-质谱法  二甲基黄  二乙基黄  粮油制品

英文关键词:gas chromatography-mass spectrometer  dimethyl yellow  methyl yellow  cereal and oilseeds products

中文摘要:

      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。

英文摘要:

      Objective To establish a method for the determination of dimethyl yellow and methyl yellow in cereal and oilseeds products by gas chromatography-mass spectrometry. Methods The samples were extracted with acetonitrile containing 1% ethylic acid, purified by oil matrix extraction tube and separated by HP-5MS column. Full scan and selected ion mode were used in mass spectrometry with external standard method for quantitative analysis. Also the effects of ways of extraction and purification on the recovery were studied. Results The average recoveries spiked at levels of 1, 10 and 25 mg/kg were in the range of 76.3%~89.3% with relative standard deviation of 3.0%~8.7%, and the limits of detection of dimethyl yellow and methyl yellow were 0.002 mg/kg and 0.001 mg/kg, respectively, which met the requirement of technical parameters for analysis. Conclusion This method is rapid and accurate, which is suitable for the determination of dimethyl yellow and methyl yellow in cereal and oilseeds products.