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| Rapid Screening and Confirmation of 123 Veterinary Drugs in Aquatic Products by On-line Cleanup/Liquid Chromatography－Quadrupole/Electrostatic Field Orbitrap High-resolution Mass Spectrometry |
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| DOI： |
| KeyWord:on-line cleanup quadrupole/electrostatic field orbitrap high-resolution mass spectrometry rapid screening aquatic products veterinary drugs |
| Author | Institution |
| OUYANG Shao-lun，LAN Cao，CHEN Wen-rui，AN Wen-jia，LIN Feng，ZHUANG Yan-jun |
Guangzhou Customs Technology Center，Guangzhou ，China
2. School of Pharmacy，Guangdong Medical University，Dongguan ，China;
3. Guangdong Provincial Key Laboratory of Radionuclides Pollution Control and Resources，Guangzhou ，China |
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| Abstract: |
| A liquid chromatography－quadrupole/electrostatic field orbitrap high-resolution mass spectrometry with on-line cleanup was established for the rapid screening of 123 veterinary drug residues in aquatic products，including fifteen types of 123 wide-range veterinary drugs，i.e．20 sulfonamides，6 macrolides，16 quinolones，12 β-agonists，17 benzimidazoles，4 tetracyclines，2 sedatives，6 hormones，4 β-lactams，1 dapsone，2 anticoccidials，2 dyes，24 glucocorticoids，1 chloramphenicols and 6 resorcylic acid lactones．The samples were extracted with acetonitrile－water（8∶2） by ultrasonic extraction，followed by an automated turbulent flow cyclone chromatography sample clean-up system．The online purification technology TurboFlow is mainly used to achieve the purpose of purification by means of diffusion and dissolution，size exclusion，etc．as it has more advantages than traditional solid phase extraction and matrix dispersion extraction．Sample extraction solution was purified and collected with a CycloneTM P column（0.5 mm × 50 mm）．The analytes were eluted from the extraction column and put into an Atlantis T3 analytical column（100 mm × 4.6 mm，3 μm） prior to chromatographic separation and detection in Full Scan/ddMS2 mode．The target compounds were monitored in both positive and negative full scan modes．The confirmatory analysis was carried out by determining the retention time and accurate masses of all compounds and fragment ions upon target MS/MS，and the external standard method was used for quantification. The total run time was within 18 min，including analytical chromatography and re-equilibration of the turboflow system．The optimization of different experimental parameters including extraction，separation and detection were evaluated separately in this paper．The developed method was validated，and good performing characteristics were obtained．The screening of analytes was performed by library searching．The method could be used for the rapid screening of 123 drugs in aquatic products by means of accurate mass of quasi-molecular ion，retention time and the secondary fragment ion spectra for confirmation. The results showed that the calibration curves of the 123 drugs were linear in their respective concentration ranges with correlation coefficients（r2） more than 0.99．The limits of quantitation were between 0.1 μg/kg and 50 μg/kg．The spiked recoveries for the analytes ranged from 53.7% to 129%，with relative standard deviations of 2.7%－19%．The developed method exhibits a great potential in the routine laboratory analysis of large number of samples belonging to different classes of compounds．Meanwhile，in comparison to traditional procedures，the automated sample clean up could ensure the rapid，effective，simple and sensitive analysis of veterinary drugs for the screening of residues in batches of aquatic products． |
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