Bước đầu xây dựng và đánh giá phương pháp xác định đồng thời độc tố vi nấm trong ngũ cốc bằng kỹ thuật sắc ký lỏng ghép nối khối phổ

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Ngôn ngữ: vie

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Thông tin xuất bản: Tạp chí Kiểm nghiệm và An toàn thực phẩm, 2022

Mô tả vật lý: tr.402-413

Bộ sưu tập: Metadata

ID: 333815

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Currently, solid phase extraction (SPE) with immunoaffinity columns is applied in most standardized methods for mycotoxin determination to purify extracts and analysis by HPLC-FLD, HPLC-UV/VIS or LC-MS/MS. Therefore, sample preparation and analysis by instruments are time-consuming and high operating costs. The novel method allow simultaneously identify nine mycotoxin compounds with selective, stable and accurate results. The new method has been evaluated through three stages including validation as requirements of CEN/TR 16059:2010 (phase 1), comparison with current standard methods (phase 2), evaluate the method using an interlaboratory comparison program (phase 3). Cereal samples were extracted by QuEChERS and analyzed by LC-MS/MS. The limit of quantitation (LOQ) was 0,5 μg/kg for each aflatoxin compound and 40 μg/kg, 25 μg/kg, 1 μg/kg, 75 μg/kg for deoxynivalenol, zearalenone, ochratoxin A, each toxin fumonisin (B1&B2), respectively. The recovery is in the range of 70-120%, relative standard deviation RSD <
20%. The novel method also gives the same results compared to the individual standardized methods, using the immunoaffinity column in the extraction stage. At the present, the method is being evaluated through an interlaboratory comparison program with two rounds: round 1 (for survey) and round 2 (official round), which is expected to be implemented in 2022.Hiện nay, các phương pháp tiêu chuẩn xác định hàm lượng độc tố vi nấm sử dụng kỹ thuật chiết pha rắn (SPE) bằng cột ái lực để làm sạch dịch chiết và phân tích trên thiết bị HPLC-FLD hoặc LC-MS/MS cho từng độc tố hoặc nhóm độc tố. Do đó, việc xử lý mẫu và phân tích trên thiết bị tốn nhiều thời gian, dẫn đến chi phí vận hành cao. Phương pháp mới có thể xác định đồng thời 09 hoạt chất mycotoxin chỉ với một lần chuẩn bị mẫu và một lần phân tích trên thiết bị, cho kết quả chọn lọc, ổn định và chính xác. Phương pháp thử đã được đánh giá qua ba giai đoạn gồm: xác nhận giá trị sử dụng theo CEN/TR 16059:2010 (giai đoạn 1), so sánh với các phương pháp tiêu chuẩn (giai đoạn 2), đánh giá phương pháp bằng chương trình so sánh liên phòng (giai đoạn 3). Các mẫu ngũ cốc được chiết bằng kỹ thuật QuEChERS, làm sạch bằng d-SPE và được phân tích trên thiết bị LC-MS/MS. Giới hạn định lượng của phương pháp (LOQ) là 0,5 μg/kg cho từng độc tố nhóm aflatoxin và 40 μg/kg, 25 μg/kg, 1 μg/kg, 75 μg/kg lần lượt cho deoxynivalenol, zearalenone, ochratoxin A, từng độc tố fumonisin (B1&B2). Hiệu suất thu hồi của phương pháp trong khoảng 70-120%, độ lệch chuẩn tương đối RSD ≤ 20%, phương pháp cho kết quả tương đương các phương pháp xác định riêng lẻ có sử dụng cột ái lực trong giai đoạn chiết mẫu. Hiện phương pháp đã được đánh giá thông qua chương trình so sánh liên phòng lần 1 (vòng khảo sát) và đang thực hiện lần 2 (vòng chính thức) dự kiến thực hiện trong năm 2022.

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