高效液相色谱-串联质谱法测定豆制品中的二甲基黄残留量

Determination of dimethyl yellow in bean products by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱串联质谱法  豆制品  二甲基黄

英文关键词:high performance liquid chromatography-tandem mass spectrometry  bean products  dimethyl yellow

中文摘要:

      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 C18 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10~500 μg/L范围内具有良好的线性关系, 在50、100和200 μg/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0.4 μg/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。

英文摘要:

      Objective To develop a method for determination of dimethyl yellow in bean products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The dried tofu samples were extracted with acetonitrile by ultrasonic extraction, and separated by Thermo C18 Acclaim RSLC column using acetonitrile water (85:15, V:V) as mobile phase for isocratic elution. Mass spectrometry (ESI+) used multiple reactions monitoring to identify the quantitative ion and qualitative ion of dimethyl yellow. Results This method could complete the separation and analysis of dimethyl yellow within 5 min. The dimethyl yellow had a good linear relationship in the range of 10~500 μg/L. The recoveries spiked at 3 levels of 50, 100 and 200 μg/L were ranged from 90.2% to 94.2% with relative standard deviations (RSD) of 0.926% (n=9), and the limit of detection (LOD) for the dimethyl yellow was 0.4 μg/kg. Conclusion The proposed method is rapid, accurate and sensitive, which is suitable for detecting dimethyl yellow in bean products.