超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查辣椒粉中10种苏丹类色素

Rapid screening of 10 Sudan dyes in paprika by ultra high performance liquid chromatography-quadrupole/electrostatic field obitrap high-resolution mass spectrometry

建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速分析辣椒粉中苏丹橙G、苏丹黄、苏丹红G、苏丹红7B、苏丹蓝Ⅱ、苏丹黑B、苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ和苏丹红Ⅳ等10种苏丹类色素的方法。样品经正己烷提取,于40℃下氮气吹干后,用1mL乙腈溶解,用ZORBAX Eclipse Plus C_(18)(3.0mm×100mm,1.8μm)分离,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱。在全扫描模式下提取10种苏丹类色素的保留时间和一级母离子精确质量数以及同位素丰度比,实现了对辣椒粉中10种苏丹类色素的快速测定;以自动触发采集的二级碎片离子精确质量数进行确证。结果表明,目标化合物的线性关系良好,相关系数(r^2)大于0.99;各化合物的检出限不大于25.0μg/kg,回收率为81.6%~109.3%,相对标准偏差为5.3%~8.9%。该方法简单、准确、快速,适用于辣椒粉中10种苏丹类色素的方法的快速筛查。

High performance liquid chromatography quadrupole/electrostatic field obitrap high resolution mass spectrometry was used to the determination of 10 Sudan dyes, i.e., Sudan Orange G. Sudan Orange. Sudan Red G. Sudan Red 7B Sudan Blue 2. Sudan Black B, Sudan Red 1. Sudan Red 2 Sudan Red 3 and Sudan Red 4 in Paprika. The samples were extracted by n-hexane, concentrated to dryness in nitrogen at 40℃ . The residue was dissolved with lmL acetonitrile, ZORBAX Eclipse Plus C18 （3.0 mm × 100 mm, 1.8 μm） was used as chromatography colomn to separat the Sudan dyes with a gradient elution of acetonitrile and 0.1% formic acid solution as the mobile phase. The retention time, accurate mass of parent ion and relative isotope abundance were used for fast screening in full scan mode, while accurate mass of fragment ions were used for comfirmation in two-stage threshold-triggered full mass scan mode.Under the optimal conditions, good linearities （r2 〉 0.99） were obtained in their respective linear ranges. The limit of detections （LODs） for 10 Sudan dyes were ≤ 25.0 μg/kg. The recoveries were in the range of 81.6% - 109.3% and the relative standard deviations （RSDs） were 5.3% - 8.9%.The method was simple, sensitive, accurate and suitable for the quantify of 10 Sudan dyes in Paprika.