超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速筛查葡萄汁中10种苏丹类色素

Rapid screening of 10 kinds of sudan dyes in grape juice by ultra performance liquid chromatography-quadrupole/electrostatic field obitrap high-resolution mass spectrometry

中文关键词:  超高效液相色谱法  四极杆/静电场轨道阱高分辨质谱法  葡萄汁  苏丹类色素  快速筛查

英文关键词:ultra performance liquid chromatography  quadrupole/electrostatic field obitrap high-resolution mass spectrometry  grape juice  sudan dyes  rapid screening

中文摘要:

      目的 建立超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速分析葡萄汁中10种苏丹类色素的方法。方法 样品经乙酸乙酯提取, 于40 ℃下旋转蒸干后, 用2 mL乙腈和0.1%甲酸水溶液(1:1, V:V)溶解, 用ZORBAX Eclipse Plus C18(3.0 mm×100 mm, 1.8 μm)超高效色谱柱分离, 以甲醇和5 mmol/L乙酸铵水溶液为流动相进行梯度洗脱。在正离子模式下测定了10种苏丹类色素; 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, 实现对葡萄汁中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 目标化合物在各自的线性范围内线性关系均良好, 相关系数(r2)大于0.99; 除苏丹红Ⅳ外, 其他化合物的检出限均不大于2.0 μg/kg; 回收率为79.1%~110.3%, 相对标准偏差为4.5%~8.3%。结论 该方法简单、准确、快速、可靠, 适用于葡萄汁中10种苏丹类色素的快速定性筛查和定量分析。

英文摘要:

      Objective To establish a rapid and simple method for the quantification of 10 kinds of sudan dyes in grape juice by ultra performance liquid chromatography-quadrupole/electrostatic field obitrap high-resolution mass spectrometry. Methods The samples were extracted by ethyl acetate, and concentrated to dryness in a rotay evaporator at 40 ℃. The residue was dissolved with 2 mL mixed solvent of ethanol and 0.1% formic acid (1:1, V:V). The ZORBAX Eclipse Plus C18 column (3.0 mm×100 mm, 1.8 μm) was used as chromatography column to separate the sudan dyes with a gradient elution of methanol and 5 mmol/L ammonium acetate aqueous solution as the mobile phase. The 10 kinds of sudan dyes were analyzed in positive mode. The retention time, accurate mass of parent ion and relative isotope abundance were used for rapid screening in full scan mode, while accurate mass of fragment ions was used for confirmation in two-stage threshold-triggered full mass scan mode. Results The linearities were good in their respective linear ranges (r2>0.99). The limits of detection (LODs) for most compounds were ≤2.0 μg/kg except for sudan red Ⅳ. The recoveries were in the range of 79.1%~110.3% and the relative standard deviations (RSDs) were 4.5%~8.3%. Conclusion The established method is simple, accurate, rapid and reliable, which is suitable for the rapid qualitative screening and quantitative analysis of 10 kinds of sudan dyes in grape juice.