Nghiên cứu xây dựng quy trình định lượng đồng thời kháng sinh fluoroquinolon trong tôm bằng phương pháp lc-ms/ms

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Tác giả: Châu Minh Vĩnh Thọ Đỗ, Huỳnh Anh Thi Huỳnh, Đoan Vi Phạm

Ngôn ngữ: Vie

Ký hiệu phân loại:

Thông tin xuất bản: Y Dược học Cần Thơ 2021

Mô tả vật lý: 45-52

Bộ sưu tập: Metadata

ID: 406703

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Tóm tắt
Chủ đề

Việc lạm dụng kháng sinh và quản lý kháng sinh thiếu kiểm soát có thể dẫn đến sự tồn lưu dư lượng của chúng trên sản phẩm thủy sản. Mục tiêu nghiên cứu: Xây dựng, thẩm định và ứng dụng quy trình định lượng đồng thời 4 kháng sinh nhóm fluoroquinolon bằng LC-MS/MS theo hướng dẫn của AOAC, EC. Đối tượng và phương pháp nghiên cứu: Enrofloxacin, ciprofloxacin, sarafloxacin, flumequin và các mẫu tôm thu thập tại Kiên Giang, xây dựng quy trình định lượng bằng hệ thống sắc ký lỏng ghép khối phổ LC-MS/MS. Kết quả: Các thông số khối phổ phù hợp xác định phân mảnh của sarafloxacin (386,02→342), ciprofoxacin (332,03→288), enrofloxacin (360,06→316), flumequin (261,98→244). Thông số sắc ký: cột GL InertSustain C18 (4,6×250mm, 5 µm), chương trình rửa giải gradient. Phương pháp có khoảng tuyến tính rộng với hệ số tương quan R2>
0,99, độ thu hồi (87,6-100,06%) và chính xác liên ngày (RSD≤7,5%) tốt, giá trị LOD và LOQ lần lượt trong khoảng 0,03-0,5ppb và 0,125-1,5ppb. Kết quả kiểm 10 mẫu tôm thị trường không có dư lượng kháng sinh phân tích vượt quá LOD của phương pháp. Kết luận: Đã xây dựng quy trình định lượng 4 kháng sinh nhóm fluoroquinolon trong tôm bằng phương pháp LC- MS/MS, thẩm định quy trình phân tích đạt yêu cầu theo hướng dẫn của EC 657/2002, kết quả phân tích trên 10 mẫu tôm thu thập tại Kiên Giang không phát hiện dư lượng của 4 kháng sinh này., Tóm tắt tiếng anh, 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 LC- MS/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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