Guo Siyan, Ding Tao, Yin Yao, Zhang Xiaoyan, Liu Han, Shen Weijian, Lin Hong, Wu Bin, Deng Xiaojun, Yi Xionghai, Yang Gongjun
Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210019, China.
College of Pharmacy, China Pharmaceutical University, Nanjing 211198, China.
Se Pu. 2019 Jan 8;37(1):15-20. doi: 10.3724/SP.J.1123.2018.08043.
A method has been developed for rapid untargeted screening and determination of unknown contaminants in aquatic products by high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry. The samples were extracted by acetonitrile, dried under nitrogen, dissolved in methanol-water (3:7, v/v), and analyzed via the full MS scan/data dependent MS mode during the screening process. The Trace Finder software was used to match the precise mass, the isotope abundance ratio, the fragment ion to search for unknown contaminants in aquatic samples. The optimized QuEChERS method is used to purify the samples when quantifying. The quantitative analyses of triazole, caffeine, and ethoxyquinoline were performed via the target-MS mode. The correlation coefficients of the three compounds in fish and shrimp samples were higher than 0.99 in the linear range of 5-1000 μg/L. The limit of detection was 1 μg/kg, and the limit of quantitation was 5 μg/kg. The average recoveries were between 70.5% and 90.9% with the relative standard deviations ranging from 5.4% to 12.8%. The screening method has the advantages of fast, accurate, and high throughput; when combined with the quantitative method, it can be used to screen and determine unknown contaminants in the actual aquatic products.
建立了一种利用高效液相色谱-四极杆/静电场轨道阱高分辨率质谱对水产品中未知污染物进行快速非靶向筛查和测定的方法。样品用乙腈萃取，氮气吹干，溶于甲醇-水（3:7，v/v），在筛查过程中通过全扫描/数据依赖扫描模式进行分析。使用Trace Finder软件匹配精确质量数、同位素丰度比、碎片离子，以在水产品样品中寻找未知污染物。定量时采用优化的QuEChERS方法净化样品。通过目标扫描模式对三唑、咖啡因和乙氧喹啉进行定量分析。在5-1000μg/L线性范围内，鱼和虾样品中三种化合物的相关系数均高于0.99。检出限为1μg/kg，定量限为5μg/kg。平均回收率在70.5%-90.9%之间，相对标准偏差在5.4%-12.8%之间。该筛查方法具有快速、准确、高通量的优点；与定量方法相结合，可用于实际水产品中未知污染物的筛查和测定。
