高效液相色谱-三重四级杆质谱法测定豆制品中二甲基黄、二乙基黄

Simultaneous determination of methyl yellow and ethyl yellow in soy products by high performance liquid chromatography-tandem mass spectrometry

建立一种同时测定豆制品中二甲基黄、二乙基黄的高效液相色谱-三重四级杆质谱(HPLC-MS/MS)方法。对提取溶剂及色谱条件进行优化,粉碎后的样品经乙腈提取,提取液以HPLC-MS/MS测定,外标法定量。二甲基黄、二乙基黄在3 min内流出并完全分离,两者在0.05~10μg/L范围内相关系数r2均大于0.999,二甲基黄在0.5~50μg/kg的加标回收率为90.0%~93.4%,RSD为0.5%~5.1%,二乙基黄在0.5~50μg/kg水平的加标回收率在84.6%~93.8%,RSD为1.1%~4.6%,检出限两者均为0.2μg/kg。该方法操作简捷、准确度和精密度高,适用于豆制品中二甲基黄、二乙基黄的检测。

To establish a method for determination of methyl yellow and ethyl yellow in soy products using high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）. According to the optimization of extraction solvent and chromatographic conditions, the samples were extracted by aeetonitrile and determined by HPLC-MS/MS using external standard method. Methyl yellow and ethyl yellow were separated completely within 3min. The linearity of methyl yellow and ethyl yellow was 0.05-10 μg/L with correlation coefficients （r^2） above 0.999. Recoveries ranged from 90.0% to 93.4% for methyl yellow at spiked levels ranging from 0.5μg/kg to 50 μg/kg, and the relative standard deviations （RSDs） were in the range of 0.5%-5.1%. As for ethyl yellow, recoveries were 84.6%-93.8% at spiked levels ranging from 0.5 μg/kg to 50 μg/kg, and the RSDs were 1.1%-4.6%. The limits of detection were 0.2μg/kg. The method is rapid, simple, accurate and sensitive. It is suitable for determination of methyl yellow and ethyl yellow in soy products.