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目的建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)测定豆制品中的二甲基黄的含量。方法豆制品经乙腈超声提取,经色谱柱Thermo C_(18)Acclaim RSLC分离,采用乙腈:水(85:15,V:V)作为流动相进行等度洗脱;质谱(electronic spray ion,ESI+)采用多离子监测模式(multiple reactions monitoring,MRM)对二甲基黄的定量离子和定性离子进行监测。结果本方法在5 min内可完成二甲基黄的分离分析。二甲基黄在10~500μg/L范围内具有良好的线性关系,在50、100和200μg/L 3个添加水平下的加标回收率为90.2%~94.2%,相对标准偏差为0.926%(n=9),方法的检出限为0.4μg/kg。结论该方法快速准确、灵敏度高,可适用于测定豆制品中二甲基黄的残留量。
Objective To establish a method for the determination of dimethyl yellow in soy products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS). Methods The soy products were extracted by acetonitrile and separated on a Thermo C_ (18) Acclaim RSLC column. The mobile phases were eluted with acetonitrile: water (85:15, V: V) Quantitative and qualitative ions of dimethyl yellow were monitored using multiple reactions monitoring (MRM). Results The separation of dimethyl yellow could be completed within 5 minutes. The calibration curve of dimethyl yellow showed good linearity in the range of 10 ~ 500 μg / L. The spiked recoveries of 90.6% ~ 94.2% with relative standard deviations of 0.926% at the three levels of 50, 100 and 200 μg / L n = 9), the detection limit of the method is 0.4μg / kg. Conclusion The method is rapid, accurate and sensitive and can be applied to the determination of dimethyl yellow residue in soy products.