超高效液相色谱-串联质谱法快速检测香辛料中13种偶氮类工业染料

Rapid detection of 13 kinds of azo industrial dyes in spices by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  香辛料  偶氮类工业染料  超高效液相色谱-串联质谱  快速检测

英文关键词:spices  azo industrial dyes  ultra performance liquid chromatography-tandem mass spectrometry  rapid detection

中文摘要:

      目的 建立超高效液相色谱-串联质谱法同时测定香辛料中非法添加的13种偶氮类工业染料(苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ、苏丹红B、罗丹明B、苏丹红G、苏丹红7B、对位红、苏丹橙G、碱性橙2、碱性橙21和碱性橙22)的方法。方法 样品用水浸润后, 经酸化乙腈(含1%乙酸)超声提取, 无水硫酸镁与氯化钠辅助净化, 浓缩后, 以乙腈-0.10%甲酸水溶液为流动相, 梯度洗脱, C18色谱柱(2.1 mm×150 mm, 1.7 μm)分离, 采用电喷雾多反应监测、正离子模式测定, 对香辛料中的13种偶氮类工业染料进行定性测定, 外标法定量。结果 13种偶氮类工业染料分别在质量浓度0.5~50.0、1~50或4~100 ng/mL范围内线性关系良好, 相关系数(r2)均大于0.99; 检出限可达1.0~10.0 μg/kg, 定量限可达3.0~30.0 μg/kg。在1倍定量限、2倍定量限与10倍定量限浓度水平的平均加标回收率为75.7%~102.4%, 相对标准偏差均低于10% (n=6)。结论 该方法前处理简便, 具有快速、准确、灵敏的优点, 适用于对香辛料中13种偶氮类工业染料的快速筛查与定量检测, 以期为偶氮类工业染料的非法添加监管提供强有力的技术支撑。

英文摘要:

      Objective To establish a method for simultaneous determination of 13 kinds of illegally added azo industrial dyes (Sudan red I, Sudan red II, Sudan red III, Sudan red IV, Sudan red B, rhodamine B, Sudan red G, Sudan red 7B, para red, Sudan orange G, basic orange 2, basic orange 21, and basic orange 22) in spices using ultra performance liquid chromatography tandem mass spectrometry. Methods After the sample was soaked with water, it was extracted with acidified acetonitrile (containing 1% acetic acid) by ultrasonic extraction, and purified with anhydrous magnesium sulfate and sodium chloride. After concentration, acetonitrile-0.10% formic acid aqueous solution was used as mobile phase, gradient elution, C18 chromatographic column (2.1 mm×150 mm, 1.7 μm) separation, electrospray multi reaction monitoring and positive ion mode determination were used to qualitatively determine 13 kinds of azo industrial dyes in spices, and external standard method was used for quantitative determination. Results The 13 kinds of azo industrial dyes showed good linear relationships within the mass concentration ranges of 0.5–50.0, 1–50, or 4–100 ng/mL, with correlation coefficients (r2) all greater than 0.99; the limits of detection could reach 1.0–10.0 μg/kg, and the limits of quantification could reach 3.0–30.0 μg/kg. The average spiked recovery rates at 1-fold, 2-fold, and 10 fold concentration levels were 75.7% to 102.4%, with relative standard deviations below 10% (n=6). Conclusion This method has the advantages of simple pretreatment, rapid, accurate, and sensitive, and is suitable for rapid screening and quantitative detection of 13 kinds of azo industrial dyes in spices, in order to provide strong technical support for the supervision of illegal addition of azo industrial dyes.