超高效液相色谱串联质谱法同时检测禽蛋中的角黄素、对位红和苏丹红Ⅰ~Ⅳ

Simultaneous determination of canthaxanthin, parared and Sudan Ⅰ-Ⅳ in egg by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱串联质谱法  固相萃取  禽蛋  角黄素  对位红  苏丹红Ⅰ~Ⅳ

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  solid phase extraction  egg  canthaxanthin  parared  Sudan Ⅰ-Ⅳ

中文摘要:

      目的 建立超高效液相色谱串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定禽蛋中角黄素、对位红和苏丹红残留量的方法。方法 禽蛋样品用乙腈超声提取, 加入氯化钠进行盐析脱水, 提取液加等体积水混合后经C18固相萃取小柱净化, 采用Waters C18色谱柱(50 mm×2.1 mm, 1.7 μm)以0.1%甲酸水和乙腈溶液为流动相梯洗脱分离, 电喷雾电离(electrospray ionization, ESI)正离子多反应监测模式进行定量分析。结果 角黄素、对位红和苏丹红质量浓度在0.2~ 100.0 μg/L范围内线性关系良好, 相关系数均在0.999以上; 在低、中、高 3个加标水平的平均回收率为80.5%~106.2%, 相对标准偏差(relative standard deviation, RSD)为0.68%~7.15%; 角黄素、对位红和苏丹红的检出限为0.2 μg/kg。结论 该方法操作简单、准确, 回收率较好, 方法检出限较低, 可应用于禽蛋中角黄素、对位红和苏丹红Ⅰ~Ⅳ的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of canthaxanthin, parared and Sudan Ⅰ-Ⅳ in egg by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Egg samples were extracted by ultrasonic with acetonitrile and dehydrated by sodium chloride, then the supernatant was diluted with equal volume of water and cleaned up by C18 SPE column. The separation was performed on Waters C18 column (50 mm×2.1 mm, 1.7 μm) by gradient elution with water containing 0.1% formic acid and acetonitrile as the mobile phases. The electrospray ionization (ESI) source in the positive mode and multiple reaction monitoring mode were used for the quantitative analysis. Results The linear concentration of canthaxanthin, parared and Sudan in the range of 0.2-100.0 μg/L was good, and the correlation coefficients were above 0.999. The average recoveries were 80.5%-106.2% with the relative standard deviation (RSD) from 0.68% to 7.15%. The limit of detection of canthaxanthin, parared and Sudan was 0.02 μg/kg. Conclusion This method is accurate and easy to operate with good recovery and low limit of detection, which is suitable for the determination of canthaxanthin, parared and Sudan Ⅰ-Ⅳ in egg.