超高效液相色谱-串联质谱法测定食品中柑橘红2号和苏丹红Ⅰ~Ⅳ染料
Simultaneous Determination of Citrus Red 2 and SudanⅠ~Ⅳ Dyes in Foodstuff by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry
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摘要: 建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定食品中柑橘红2号和苏丹红Ⅰ~Ⅳ染料的检测方法。样品采用乙腈-氯化钠体系提取,NH2固相萃取柱净化,经超高效液相色谱分离,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,三重四极杆质谱电喷雾电离(ESI+)检测,多反应监测模式(MRM),基质外标法定量。结果表明,柑橘红2号和苏丹红Ⅰ~Ⅳ 5种成分在2~40 ng/mL范围内线性关系良好,决定系数(R2)为0.998。低中高三个添加水平下,5种染料加标回收率在80.7%~114%之间,相对标准偏差范围<8.6%。方法检出限(S/N ≥ 3)为5.0 μg/kg,定量限(S/N ≥ 10)为10.0 μg/kg。该方法简便、快捷、高效、灵敏度高,适用于柑橘类水果、蜜饯、辣椒油、火锅底料及肉制品等多种食品基质中柑橘红2号和苏丹红Ⅰ~Ⅳ染料的同时检测。Abstract: A method for determination of Citrus Red 2 and SudanⅠ~Ⅳ in food by ultra performance liquid chromatography-tandem mass spectrometry was established. The samples were extracted with acetonitrile sodium chloride system and purified by NH2 column. The separation was carried out by ultra performance liquid chromatography(UPLC). The target compounds were detected by MS/MS system with electrospray ionization(ESI)under multiple reaction monitoring(MRM)mode. Results showed that,the calibration curves of 5 illegal dyes showed good linearity in 2~40 ng/mL with determination coefficients 0.998. The average recoveries ranged from 80.7% to 114% at three spiking levels with RSD<8.6%. The limit of detection(LOD)and the limit of quantitation(LOQ)of Citrus Red 2 and SudanⅠ~Ⅳ in five matrics were 5.0 and 10.0 μg/kg,respectively. This rapid and sensitive method could be applied for quantitative determination of Citrus Red 2 and SudanⅠ~Ⅳ in foodstuff.
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