SIMULTANEOUS DETERMINATION OF FLUOROQUINOLON IN SHRIMP BY LC-MS/MS

Huynh Anh Thi Huynh1, Doan Vi Pham2, Chau Minh Vinh Tho Do1,
1 Can Tho University of Medicine and Pharmacy
2 Tay Do University

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Abstract

  Background: The overuse and the lack of the management of antibiotic can lead to the persistence of their residues on aquaculture products. Objectives: To develop, validate a procedure for simultaneous quantitative analaysis of fluoroquinolon in shrimp samples by LC-MS/MS according to AOAC, EC guidelines; procedure application for shrimp samples in Kien Giang province. Materials and methods: Enrofloxacin, ciprofloxacin, sarafloxacin, flumequin and shrimp samples collected in Kien Giang province, develop simultaneous determination procedure by LCMS/MS system. Results: The suitable mass spectrometry parameters were used to quantify the fragment ion of sarafloxacin (386.02→342), ciprofoxacin (332.03→288), enrofloxacin (360.06→316), flumequin (261.98→244). Suitable chromatographic parameters: GL InertSustain C18 (4.6 × 250 mm, 5 µm), gradient elution program. The method was validated with a wide linear range with correlation coefficient R2>0.99, good accuracy (87.6–100.06%) and inter-day precision (RSD<7.5%), LOD and LOQ values were 0.03-0.5ppb and 0.125-1.5ppb, respectively. The antibiotic residues of 10 shrimp samples were not exceeded the LOD of method. Conclusion: Developed the analytical procedure for 4 fluoroquinolon antibiotics in shrimp by LC-MS/MS, the analytical procedure was validated according to EC 657/2002 guidline, the analysis results on 10 shrimp samples collected in Kien Giang did not detect residues of these 4 antibiotics. 

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References

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