色谱

色谱 ›› 2019, Vol. 37 ›› Issue (1): 15-20.DOI: 10.3724/SP.J.1123.2018.08043

• 特别策划：南京海关动植物与食品检测中心专栏 • 上一篇    下一篇

高效液相色谱-四极杆/静电场轨道阱高分辨质谱对水产品中未知污染物的非定向快速筛查与测定

郭思言1,2, 丁涛1, 殷耀1, 张晓燕1, 柳菡1, 沈伟健1, 林宏1, 吴斌1, 邓晓军3, 伊雄海3, 杨功俊2   

  1. 1. 南京海关动植物与食品检测中心, 江苏 南京 210019;
    2. 中国药科大学药学院, 江苏 南京 211198;
    3. 上海海关动植物与食品检验检疫技术中心, 上海 200135
  • 收稿日期:2018-08-28 出版日期:2019-01-08 发布日期:2014-11-29
  • 通讯作者: 丁涛E-mail:953580528@qq.com.
  • 基金资助:

    政府间国际科技创新合作重点专项（2017YFE0110800）.

Rapid untargeted screening and determination of unknown contaminants in aquatic products by high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

GUO Siyan1,2, DING Tao1, YIN Yao1, ZHANG Xiaoyan1, LIU Han1, SHEN Weijian1, LIN Hong1, WU Bin1, DENG Xiaojun3, YI Xionghai3, YANG Gongjun2   

  1. 1. Animal, Plant and Food Inspection Center, Nanjing Customs, Nanjing 210019, China;
    2. College of Pharmacy, China Pharmaceutical University, Nanjing 211198, China;
    3. Animal, Plant and Food Inspection & Quarantine Center, Shanghai Customs, Shanghai 200135, China
  • Received:2018-08-28 Online:2019-01-08 Published:2014-11-29
  • Supported by:

    Key Projects of International Scientific and Technological Innovation Cooperation Between Governments(No. 2017YFE0110800).

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摘要：

建立了高效液相色谱-四极杆/静电场轨道阱高分辨质谱对水产品中污染物的非定向快速筛查与测定的方法。筛查时样品用乙腈提取、氮气浓缩吹干、甲醇-水溶液定容，采用全扫描数据依赖二级扫描模式进样分析。利用Trace Finder软件对水产样品中未知污染物的精确质量数、同位素丰度比、二级碎片离子进行数据库检索匹配。定量时样品采用优化的QuEChERS方法净化，对筛查过程确认的三环唑、咖啡因和乙氧基喹啉3种污染物进行目标离子二级扫描模式定量分析。鱼和虾中3种化合物在5~1000 μg/L范围内线性关系良好，相关系数均大于0.99；方法检出限（LOD）为1 μg/kg，定量限（LOQ）为5 μg/kg，平均回收率为70.5~90.9%，相对标准偏差为5.4%~12.8%。筛查方法具有快速、准确、高通量等优点，结合定量方法能够用于实际水产品中未知污染物的筛查与测定。

关键词: 非定向筛查, 高分辨质谱, 高效液相色谱, 水产品, 污染物

Abstract:

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 MS2 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-MS2 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.

Key words: aquatic products, contaminants, high performance liquid chromatography (HPLC), high resolution mass spectrometry (HRMS), untargeted screening

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