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8267596 
Journal Article 
UPLC-MS/MS同时测定水产品中 4种丁香酚类麻醉剂残留量 
Ni, ZF; Gu, Y; Feng, YW; Xue, QH; Wang, Q 
2018 
Chinese Society for Mass Spectrometry 
39 
4 
451-458 
Chinese 
The method for simultaneous determination of 4 eugenol derivatives anesthetics residues in aquatic products was developed by solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The influences of extraction procedures, chromatographic conditions and mass spectrometry conditions were investigated. The optimal solid phase extraction experiment conditions were as follows: the aquatic samples were extracted with 5 mL hexane twice, supernatant was combined and centrifuged at 6 000 r/min, enriched by nitrogen blowing at 35 ℃, mixed with 3 mL 40% methanol, cleaned up by solid phase column of hydrophilic-lipophilic balance (HLB) cartridge, then rinsed by 3 mL 40% methanol, eluted by 2 mL methanol, dried with nitrogen gas at 35 ℃. The chromatographic separation was performed within 13.0 min on an Agilent ZORBAX Eclipse Plus C18 column (50 mm×2.1 mm×1.8 μm). Formic acid played a key role in mobile phase as modifier to improve the ionization efficiency of methyleugenol and methylisoeugenol. The flow rate was 0.30 mL/min. An Agilent 6470 Triple Quadrupole mass spectrometer (QQQ-MS) was operated in the positive and negative ion modes at the same time using multiple reaction monitoring (MRM) for qualitative and quantitative analysis of 4 eugenol derivatives which were quantitated with an external standard method. The QQQ-MS conditions were optimized including ionization mode, precursor ion, product ion, fragmentor voltage, and collision energy. The limits of quantitation for eugenol and isoeugenol are 2.5 μg/kg while the limits of quantitation for methyleugenol and methylisoeugenol are 1.0 μg/kg. The linear correlation coefficient (R2) is over 0.996 in the range of 1-200 μg/L for eugenol derivatives' concentrations. The average recoveries for eugenol derivatives are 77.6%-111.4% with RSDs of 2.7%-9.1%. This method is precise, selective and reliable, and has been successfully applied for detection and determination of eugenol, isoeugenol, methyleugenol and methylisoeugenol simultaneously in batch sample of aquatic products. © 2018, Science Press. All right reserved. 
Eugenol; Isoeugenol; Methyleugenol; Methylisoeugenol; Solid phase extraction; Ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)