Xác định đồng thời một số kháng sinh nhóm diệt cầu trùng trong thực phẩm bằng phương pháp sắc ký lỏng khối phổ hai lần (LC-MS/MS)=Simultaneous determination of some coccidiostat antibiotics in food by liquid chromatography tandem mass spectrometry (LC-MS/MS)

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Ngôn ngữ: vie

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Thông tin xuất bản: Tạp chí Kiểm nghiệm và An toàn thực phẩm, 2024

Mô tả vật lý: tr.329-342

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ID: 481751

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Coccidiostats (anticoccidial antibiotics) are veterinary drugs widely used for the prevention and treatment of coccidiosis, especially in poultry farming. The illegal use of anticoccidial antibiotics, in the wrong dosage and duration, can lead to antibiotic residues in animal products and harm the health of consumers. In this study, a highly sensitive and accurate liquid chromatography-tandem mass spectrometry method was developed for the simultaneous analysis of anticoccidial antibiotics (diclazuril, nicarbazin, robenidin and salinomycin) in food. Samples were extracted using the QuEChERS method with acetonitrile (ACN) as the extraction solvent and cleaned with C18 adsorbent. The cleaned extracts were analyzed on an LC-MS/MS system with a C18 reversed-phase chromatography column (2.1 x 150 mm, 3.5 µm) and corresponding pre-column. The mobile phase used was 0.1% HCOOH in water and methanol (MeOH), the flow rate was 0.5 mL/min. The method had good specificity, the linear range was established in the range of 10-100 ng/mL, the correlation coefficient R2 >
0.998. The method recovery was in the range of 81-109% and the relative standard deviation (RSD%) was in the range of 1.77-10.13% for milk and meat samples. The limit of quantification and limit of detection of the method for four coccidiostat antibiotics were 3.0 µg/kg and 10 µg/kg, respectively. The method was applied to analyze the content of these four antibiotics in 31 food samples (meat and meat products, milk and dairy products) randomly purchased in Hanoi. The results did not detect four coccidiostat antibiotics in all 31 samples, initially showing that the residual contamination of coccidiostat antibiotics is basically safely controlled.Coccidiostats (kháng sinh diệt cầu trùng) là loại thuốc thú y được sử dụng rộng rãi để phòng ngừa và điều trị bệnh cầu trùng, đặc biệt là trong chăn nuôi gia cầm. Việc sử dụng kháng sinh diệt cầu trùng trái phép, không đúng liều lượng và thời gian có thể dẫn tới việc tồn dư kháng sinh trong các sản phẩm có nguồn gốc động vật và gây hại tới sức khỏe người tiêu dùng. Trong nghiên cứu này, phương pháp sắc ký lỏng khối phổ hai lần với độ nhạy tốt và chính xác cao đã được phát triển để phân tích đồng thời các kháng sinh nhóm diệt cầu trùng (diclazuril, nicarbazin, robenidin và salinomycin) trong thực phẩm. Mẫu được chiết bằng phương pháp QuEChERS với dung môi chiết là acetonitrile (ACN) và làm sạch bằng chất hấp phụ C18. Dịch chiết sau khi làm sạch được phân tích trên hệ thống LC-MS/MS với cột sắc ký pha đảo C18 (2,1 x 150 mm, 3,5 µm) và tiền cột tương ứng. Pha động được sử dụng là HCOOH 0,1% trong nước và methanol (MeOH), tốc độ dòng là 0,5 mL/phút. Phương pháp có độ đặc hiệu tốt, khoảng tuyến tính được xây dựng trong khoảng 10 - 100 ng/mL, hệ số tương quan R2 >
0,998. Độ thu hồi của phương pháp nằm trong khoảng 81 - 109% và độ lệch chuẩn tương đối (RSD%) nằm trong khoảng 1,77 - 10,13% đối với nền mẫu sữa và thịt. Giới hạn định lượng và giới hạn phát hiện của phương pháp đối với 04 chất kháng sinh nhóm diệt cầu trùng tương ứng là 3,0 µg/kg và 10 µg/kg. Phương pháp được áp dụng để phân tích hàm lượng 04 chất kháng sinh này trong 31 mẫu thực phẩm (thịt và sản phẩm từ thịt, sữa và sản phẩm từ sữa) được mua ngẫu nhiên trên địa bàn Hà Nội. Kết quả không phát hiện 04 chất kháng sinh nhóm diệt cầu trùng trong tất cả 31 mẫu, bước đầu cho thấy việc tồn dư ô nhiễm kháng sinh nhóm cầu trùng cơ bản được kiểm soát an toàn.

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