固相萃取-超高效液相色谱法同时测定辣椒制品中非法添加苏丹红染料

Simultaneous determination of Sudan dyes illegally added into chili products by solid-phase extraction-ultra performance liquid chromatography

中文关键词:  苏丹红  固相萃取  超高效液相色谱法  辣椒制品  非法添加

英文关键词:Sudan dyes  solid-phase extraction  ultra performance liquid chromatography  chili products  illegally added

中文摘要:

      目的 建立固相萃取-超高效液相色谱法同时测定辣椒干、辣椒酱、辣椒油等辣椒制品中非法添加的4种苏丹红染料(苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ)的方法。方法 样品经正己烷超声提取, 提取液经ProElutTMSDH苏丹红专用柱净化富集, 采用Agilent ZORBAX Eclipse Plus C18柱(4.6 mm×100 mm, 3.5 μm), 以乙腈-水为流动相梯度洗脱分离, 二极管阵列检测器测定, 检测波长为500 nm (苏丹红Ⅰ、Ⅱ、Ⅲ)、520 nm (苏丹红Ⅳ), 利用保留时间和光谱图定性, 外标法定量。结果 苏丹红Ⅰ~Ⅳ可在6.5 min内实现完全分离, 4种目标物在0.1~5.0 μg/mL范围内线性关系良好, 相关系数(r)均大于0.9999; 检出限为8~15 μg/kg, 定量限为26~ 48 μg/kg。在0.05、0.3、1.5、4.0 mg/kg的平均加标回收率为84.4%~98.5%, 相对标准偏差为0.3%~5.7% (n=6)。结论 该方法操作简便、准确、快速、灵敏、稳定, 易推广应用于常规实验室辣椒制品中非法添加苏丹红染料的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of 4 kinds of Sudan red dyes (Sudan red Ⅰ, Sudan red Ⅱ, Sudan red Ⅲ, Sudan red Ⅳ) illegally added into chili products by solid-phase extraction combined with ultra performance liquid chromatography. Methods The samples were extracted by ultrasound with n-hexane, purified and enriched with ProElutTMSDH special extraction cartridge column. The chromatographic separation was performed on an Agilent ZORBAX Eclipse Plus C18 column (4.6mm×100mm, 3.5μm) by gradient elution with water and acetonitrile as mobile phase. Sudan dyes were detected at the wavelength of 500nm (Sudan Ⅰ, Ⅱ, Ⅲ) and 520nm (Sudan Ⅳ) by diode array detector. Retention time and spectra characterization were used for qualitative analysis, and external standard method was used for quantification. Results Sudan Ⅰ-Ⅳ were separated completely in 6.5 min, the 4 kinds of targets had a good linear relationship in the range of 0.1?5.0 μg/mL, and the correlation coefficients (r) were all greater than 0.9999. The limits of detection were 8?15 μg/kg, and the limits of quantitation were 26?48 μg/kg. When the addition amount was 0.05, 0.3, 1.5 and 4.0mg/kg, the average recovery rates were 84.4%?98.5%, with relative standard deviations of 0.3%?5.7% (n=6). Conclusion This method is simple, accurate, rapid, sensitive and stable, and can be used for the analysis of Sudan dyes illegally added into chili products at routine labratory.