Analytical and Bioanalytical Chemistry ( IF 3.8 ) Pub Date : 2018-05-11 , DOI: 10.1007/s00216-018-1124-5 Cong Kong , Yang Wang , Yuanfei Huang , Huijuan Yu
A quick screening method of more than 200 pharmaceutical and other residues in aquatic foods based on ultrahigh-performance liquid chromatography–quadrupole-Orbitrap mass spectrometry (UHPLC-Q/Orbitrap MS) was established. In this method, after the addition of 200 μL of 1 M EDTA-Na2, 2 g of each sample homogenate was extracted successively with 10 mL of acetonitrile and 10 mL of ethyl acetate. The extracts were combined, dried under nitrogen flow, and redissolved in 0.1% formic acid in acetonitrile/water (4:6, v/v) for analysis. The prepared samples were analyzed by UHPLC- Q/Orbitrap MS system in Full MS/ddMS2 (full-scan data-dependent MS/MS) mode. Compound identification was performed through comparison of the sample data with the database for standard chemicals, including the retention time, precursor ion, product ions, and isotope pattern for all 206 compounds. Five different aquatic food matrices (carp, shrimp, crab, eel, and mussel) spiked with the analytes at 1, 10, and 50 ng/g were evaluated to assess recoveries, precision, matrix effects, stability, and detection limits using the method. UHPLC analyses required 25 min, and 178–200 analytes met identification criteria at 50 ng/g depending on the matrix. Furthermore, practical application of this method for real samples displayed strong screening capability.
中文翻译:
超高效液相色谱-四极杆-Orbitrap质谱法对水产品中的> 200种药物和其他残留物进行多类筛查
建立了一种基于超高效液相色谱-四极杆-Orbitrap质谱(UHPLC-Q / Orbitrap MS)的快速筛查水产品中200多种药物和其他残留物的方法。在该方法中,添加200μL1 M EDTA-Na 2后,分别用10 mL乙腈和10 mL乙酸乙酯萃取2 g样品匀浆。合并萃取液,在氮气流下干燥,并重新溶于0.1%甲酸的乙腈/水(4:6,v / v)溶液中进行分析。制备的样品通过UHPLC-Q / Orbitrap MS系统在Full MS / ddMS 2中进行分析(完全扫描数据相关的MS / MS)模式。通过将样品数据与标准化学品的数据库进行比较来进行化合物鉴定,包括所有206种化合物的保留时间,前体离子,产物离子和同位素模式。评估了以1、10和50 ng / g的分析物加标的五种不同的水生食品基质(鲤鱼,虾,蟹,鳗鱼和贻贝),以评估回收率,精度,基质效应,稳定性和检测限。UHPLC分析需要25分钟,根据基质,178–200种分析物满足50 ng / g的鉴定标准。此外,该方法在实际样品中的实际应用显示出强大的筛选能力。