气相色谱-质谱法检测豆制品中的二甲基黄

Determination of Dimethyl Yellow in Bean Products by Gas Chromatography–Mass Spectrometry

建立气相色谱– 质谱法测定豆制品中二甲基黄的方法.考察了不同样品前处理方法对回收率的影响.试样用dSPE 纯化管超声净化后,以10 mL 乙腈提取.样品溶液经毛细管气相色谱柱HP–5MS 分离,以质谱检测器（MSD） 测定其中的二甲基黄含量.二甲基黄的质量浓度在0.05-1.5 ng/mL 范围内与响应值呈良好的线性关系,相关系数r=0.999 1,检出限为0.005 mg/kg.加标水平为0.005-1.0 mg/kg 时的平均回收率为70%-88%,测定结果的相对标准偏差为2.5%-8.0%（n=6）.该方法净化效果好,灵敏度高,适合于豆制品中二甲基黄的检测.

A method for determination of dimethyl yellow in bean products with GC–MS was eastablished. The samples were extracted by 10 mL acetonitrile with dSPE purified column. The sample solution was separated by HP–5 MS, then dimethyl yellow in it was detected by MSD. The mass concentration of dimethyl yellow was linear with response value in the range of 0.05–1.5 ng/mL with correlation coefficient of 0.999 1, the detection limit was 0.005 mg/kg. The recoveries of dimethyl yellow were in the range of 70%–88% at spiked levels of 0.005–1.0 mg/kg,the relative standard deviation of detection results were 2.5%–8.0%(n=6). The method has good sensitivity and purification effect, which is suitable for the determination of dimethyl yellow in bean products.