基质分散固相萃取-高效液相色谱-轨道离子 阱高分辨质谱法对水产品中12种禁用化合物的快速筛查和确证

Rapid screening and confirming of 12 kinds of prohibited compounds in aquatic products by QuEChERS-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

中文关键词:  基质分散固相萃取  高效液相色谱-轨道离子阱高分辨质谱  水产品  禁用化合物

英文关键词:QuEChERS  high performance liquid chromatography quadrupole/electrostatic field orbitrap high resolution mass spectrometry  aquatic products  prohibited compounds

中文摘要:

      目的 建立基质分散固相萃取-轨道离子阱高分辨质谱法快速筛查、确证水产品中12种禁用化合物。方法 采用乙腈提取, PSA(乙二胺-N-丙基填料)以及C18净化。选用0.1%甲酸(V:V)(A)和0.1%甲酸-乙腈(V:V)(B)作为流动相洗脱正模式监测的化合物; 选用0.05%氨水(V:V)(A)和乙腈(B)作为流动相洗脱负模式监测的化合物; 采用轨道离子阱高分辨质谱仪, 在全扫描(full MS)-数据依赖扫描(ddMS2)模式下进行检测。结果 本方法的定量限为0.1~1 μg/kg; 在鱼、虾、蟹、贝4种基质中, 12种化合物的平均回收率分别为84.5%~104%、90.9%~107%、91.5%~105%、93.8%~103%, 相对标准偏差(relative standard deviation, RSD)均小于20%。 结论 本方法快速、简便、灵敏度高, 适用于水产品中多种禁用化合物的快速筛查和确证。

英文摘要:

      Objective To establish a method for screening and confirming 12 kinds of prohibited compounds in aquatic products by QuEChERS-high performance liquid chromatography-quadrupole/electrostatic field orbitraphigh resolution mass spectrometry (HPLC-Q/Orbitrap MS). Methods Samples were extracted by acetonitrile, purified by PSA and C18. Positive mode compounds were eluted by 0.1% formic acid (V:V) (A) and 0.1% formic acid acetonitrile (V:V) (B), and negative mode compounds were eluted by 0.05% ammonia (V:V) (A) and acetonitrile (B). The analytes were determined by quadrupole/electrostatic field orbitrap high resolution mass spectrometry in full-MS and data-dependent scan (ddMS2) mode. Results The limits of quantitation (LOQ) were 0.1~1 μg/kg, and the average recoveries of the 12 compounds in fish, shrimp, crab and shell were 84.5%~104%, 90.9%~107%, 91.5%~105%, 93.8%~103%, respectively, and the relative standard deviation (RSD) were less than 20%. Conclusion This method is simple, rapid, sensitive and suitable for rapid screening and confirming of the 12 kinds of prohibited compounds in aquatic products.