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

作　　者：刘俊 朱吕 陆春燕 徐秋生 LIU Jun;ZHU Lv;LU Chun-Yan;XU Qiu-Sheng(Pinghu Food and Drug Inspection Center,Pinghu 314200,China)

机构地区：[1]平湖市食品药品检测中心,平湖314200

出　　处：《食品安全质量检测学报》2018年第18期4953-4958,共6页Journal of Food Safety and Quality

摘　　要：目的建立超高效液相色谱串联质谱法(ultraperformanceliquidchromatography-tandemmass 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,加入氯化钠迚行盐析脱水,提取液加等体积水混合后经C_(18) 固相萃取小柱净化,采用Waters C_(18)色谱柱(50mm×2.1mm,1.7μm)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迚行定量分析。结果角黄素、对位红和苏丹红质量浓度在0.2～100.0μg/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0.2μg/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。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 supematant was diluted with equal volume of water and cleaned up by Cls SPE column. The separation was performed on Waters Cls column （50 min×2.1 mm, 1.7μm） 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 ×g/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 0.02μg/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.

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 

分 类 号：O657.63[理学—分析化学] TS253.7[理学—化学]