【摘要】 建立了禽蛋及其制品中4种苏丹红染料(苏丹红Ⅰ,Ⅱ,Ⅲ和Ⅳ)残留量的固相萃取/超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。样品经正己烷超声提取,上清液经苏丹红专用SPE柱净化,采用Waters CORTECSTMUPLCC18(2.1 mm×100 mm,1.7μm)柱以5 mmol/L乙酸铵溶液-0.2%甲酸和乙腈为流动相梯度洗脱分离,电喷雾电离(ESI)正离子多反应监测模式(MRM)进行测定,内标法定量。结果表明,苏丹红Ⅰ~Ⅳ在0.5~20μg/L范围内线性关系良好,相关系数均大于0.999;在低、中、高3个加标水平的平均回收率为80.0%~104.2%,相对标准偏差为4.2%~10.9%。方法的检出限(LOD)为0.26~0.35μg/kg,定量下限(LOQ)为0.9~1.2μg/kg。该方法操作简便、准确、快速、灵敏,可用于禽蛋和蛋制品中苏丹红染料的检测分析。更多还原

【Abstract】 A solid-phase extraction combined with ultra performance liquid chromatography- tandem mass spectrometric method was established for the simultaneous determination of Sudan Red dyes( Sudan RedⅠ,Ⅱ,Ⅲ and Ⅳ) in poultry eggs and its products. The samples were ultrasonically extracted with n-hexane,and then the supernatant was purified with tonyred dedicated SPE column.The chromatographic separation was performed on a Waters CORTECSTMUPLC  C18( 2. 1 mm × 100 mm,1. 7 μm) by gradient elution with 5 mmol / L ammonium acetate solution containing 0. 2% formic acid and acetonitrile as mobile phase. The electrospray ionization( ESI) source in the positive mode and multiple- reaction monitoring( MRM) mode were used for the quantitative analysis by the internal standard. The results showed that the calibration curves for four Sudan Red dyes were in good linearities in the range of 0. 5- 20 μg / L with correlation coefficients more than 0. 999. The average recoveries ranged from 80. 0% to 104. 2% with relative standard deviations( RSDs) of 4. 2%-10. 9% in low,medium and high standard addition levels. The limits of detection( LODs) and the limits of quantitation( LOQs) of this method were in the ranges of 0. 26- 0. 35 μg / kg and 0. 9- 1. 2μg /kg for four analytes,respectively. The method was simple,accurate,rapid and sensitive,and could be used for the analysis of Sudan Red dyes in poultry eggs and egg products.更多还原