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Rapid and sensitive determination of Sudan dyes in hot chilli products by solid-phase extraction directly combined with time-of-flight mass spectrometry

机译:直接结合飞行时间质谱的固相萃取快速,灵敏地测定辣椒产品中的苏丹红

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A novel method based on combination of a solid-phase extraction (SPE) with humic acid-bonded silica (HAS) as sorbent with electrospray ionization quadrupole time-of-flight mass spectrometry (ESI-QTOF MS) was developed for rapid and sensitive determination of four Sudan dyes in hot chilli products. A SPE procedure was optimized for the improvement of extraction efficiency and the removal of the matrix interferences such as the pigments and lipophilic compounds from hot chilli products. Under the optimum conditions, the desorbed analytes from the SPE sorbent allowed direct analysis by ESI-QTOF MS without time-consuming chromatographic separation. In the positive ion mode and MS/MS mode, linearities for concentration ranges of two orders of magnitude were obtained with the correlation coefficients (R2) greater than 0.9990; the limit of detection (LOD) and limit of quantification (LOQ) for four Sudan dyes were in the ranges of 1.1–4.3 and 3.8–14.3 ng g?1 depending on matrices, respectively. The recoveries of four Sudan dyes in two matrices ranged from 85.6 to 119.7%, with relative standard deviations (n = 4, 3) less than 11.3% and 11.6%. The developed method was successfully applied for the determination of Sudan dyes in six hot chilli products and the positive samples were confirmed with a high number of identification points (IPs) according to IPs system defined by Commission Decision 2002/657/EC...
机译:建立了一种以固相萃取(SPE)和腐殖酸键合二氧化硅(HAS)为吸附剂并结合电喷雾电离四极杆飞行时间质谱(ESI-QTOF MS)的新方法,用于快速,灵敏的测定辣椒产品中包含四种苏丹染料。对SPE程序进行了优化,以提高提取效率并消除热辣椒产品中的基质干扰物,例如色素和亲脂性化合物。在最佳条件下,从SPE吸附剂中解吸的分析物可以通过ESI-QTOF MS直接分析,而无需进行费时的色谱分离。在正离子模式和MS / MS模式下,相关系数(R2)大于0.9990,获得了两个数量级浓度范围的线性。四种苏丹染料的检出限(LOD)和定量限(LOQ)分别在1.1–4.3和3.8–14.3 ng g?1范围内,具体取决于基质。在两种基质中四种苏丹染料的回收率在85.6至119.7%之间,相对标准偏差(n = 4、3)分别小于11.3%和11.6%。所开发的方法已成功应用于六种辣椒产品中苏丹红的测定,并且根据委员会决议2002/657 / EC所定义的IP系统,以大量的识别点(IP)确认了阳性样品。

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