Zhang Yantu, Zhang Zhujun, Sun Yonghua
Department of Chemistry, School of Chemistry and Materials Science, Shaanxi Normal University, Xi'an 710062, China.
J Chromatogr A. 2006 Sep 29;1129(1):34-40. doi: 10.1016/j.chroma.2006.06.028. Epub 2006 Aug 17.
The determination of four Sudan dyes by means of high-performance liquid chromatography (HPLC) with chemiluminescence (CL) detection was proposed. The method was based on the enhancement effect of Sudan dyes on the chemiluminescence reaction between luminol and BrO-, which was on-line electrogenerated by constant current electrolysis. The separation was carried out on Nucleosil RP-C18 column (250 mm x 4.6 mm i.d., 5 microm, pore size, 100 A) at 35 degrees C. The mobile phase consisted of a V (methanol): V (0.2% aqueous formic acid) = 90:10 solution. At a flow-rate of 1.0 ml min(-1), the total run time was 25 min. The effects of several parameters on the HPLC resolution and CL emission were studied systematically. For the four Sudan dyes, the limits of detection (LOD) at a signal-to-noise of 3 ranged from 4 to 8 microg kg(-1) and the limits of quantification (LOQ) at a signal-to-noise of 10 ranged from 13 to 27 microg kg(-1). The relative standard deviations (RSD) of intra-and inter-day precision were below 4.4%. The average recoveries for all four Sudan dyes (spiked at the levels of 1.0 and 1.5 mg kg(-1)) in chilli tomato sauce and hot chilli pepper ranged from 94% to 105%, and the relative standard deviations of the quantitative results were from 2.5 to 4.2%. The proposed method had been successfully applied to the determination of four Sudan dyes in hot chilli products.
提出了一种采用高效液相色谱（HPLC）结合化学发光（CL）检测法测定四种苏丹红染料的方法。该方法基于苏丹红染料对鲁米诺与溴酸根之间化学发光反应的增强作用，溴酸根通过恒流电解在线电生成。分离在35℃下于Nucleosil RP - C18柱（250 mm×4.6 mm内径，5μm粒径，100 Å孔径）上进行。流动相由V（甲醇）:V（0.2%甲酸水溶液）= 90:10的溶液组成。流速为1.0 ml min⁻¹时，总运行时间为25分钟。系统研究了几个参数对HPLC分离度和CL发射的影响。对于四种苏丹红染料，信噪比为3时的检测限（LOD）在4至8 μg kg⁻¹之间，信噪比为10时的定量限（LOQ）在13至27 μg kg⁻¹之间。日内和日间精密度的相对标准偏差（RSD）均低于4.4%。在辣椒酱、番茄酱和干辣椒中添加水平为1.0和1.5 mg kg⁻¹的所有四种苏丹红染料的平均回收率在94%至105%之间，定量结果的相对标准偏差为2.5%至4.2%。该方法已成功应用于辣椒制品中四种苏丹红染料的测定。
