Xác định đồng thời bốn dạng phosphate trong thực phẩm bằng phương pháp sắc ký trao đổi ion

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

Mô tả vật lý: tr.132-143

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Nhóm phosphate là một nhóm phụ gia thực phẩm được sử dụng phổ biến bởi khả năng làm tăng tính giữ nước, cải thiện cấu trúc, giữ màu và hương vị của các sản phẩm được chế biến từ thịt, cá, sữa, bánh nướng và nước giải khát. Phương pháp sắc ký trao đổi ion nhanh và có độ tin cậy cao đã được phát triển để xác định đồng thời một số dạng phosphate (acid ortho-phosphoric
pyrophosphate, triphosphate, hexametaphosphate) trong thực phẩm. Mẫu phân tích được chiết bằng nước deion tại nhiệt độ 25 ± 5oC trong 30 phút. Dung dịch mẫu được xác định bằng sắc ký trao đổi ion với các điều kiện: cột Dionex IonPacTM AS11 (4 x 250 mm, 9 µm) và tiền cột Dionex IonPaxTM AG11 (4 x 50 mm, 9 µm), dung dịch rửa giải là dung môi KOH, nước deion với chương trình gradient nồng độ thay đổi từ 20 mM đến 80 mM. Tốc độ dòng là 1 mL/phút. Phương pháp có độ đặc hiệu tốt, đường chuẩn của bốn chất có hệ số tương quan R2 >
0,9999 và độ lặp lại, độ thu hồi đạt yêu cầu của AOAC. Giới hạn phát hiện (LOD) của mỗi chất trong nhóm phosphate lần lượt là 12 mg/kg và 40 mg/kg. Phương pháp đã được áp dụng để xác định đồng thời một số dạng phosphate trong 50 mẫu thực phẩm cho kết quả: 15/50 mẫu phát hiện hàm lượng pyrophosphate, 2/50 mẫu phát hiện hàm lượng triphosphate, 18/50 mẫu phát hiện hexametaphosphate và 44/50 mẫu phát hiện acid ortho-phosphoric. Trong đó, 6/50 mẫu không phát hiện cả bốn chất. Các sản phẩm phát hiện nhóm phosphate có hàm lượng tính theo Phospho trong các sản phẩm dao động từ 67,9 mg/kg đến 2499 mg/kg.The phosphate group is a group of food additives commonly used for moisturizing, improving the structure, and retaining the color and flavor of products prepared from meat, fish, milk, baked goods, and beverages. A reliable and fast ion exchange chromatography method developed for the simultaneous determination of several forms of phosphate (orthophosphoric acid
pyrophosphate, triphosphate, and hexametaphosphate) in food. Samples were extracted with deionized water at a temperature of 25 ± 5oC for 30 minutes. The extracts were determined by ion exchange chromatography under the conditions: Dionex IonPacTM AS11 column (4 x 250 mm, 9 µm) and Dionex IonPaxTM AG11 column (4 x 50 mm, 9 µm) with the gradient program of KOH concentration from 20 mM to 80 mM. The flow rate is 1 mL/min. The method has good specificity, the calibration curves of the four substances have correlation coefficient values R2 >
0.9999, repeatability and recovery meet the requirements of AOAC. The detection limits (LOD) and quantification limit (LOQ) of each substance in the phosphate group are 12 mg/kg and 40 mg/kg, respectively. The method was applied to simultaneously determine several forms of phosphate in 50 food samples: 15/50 samples detected pyrophosphate, 2/50 samples detected triphosphate, 18/50 samples detected hexametaphosphate and 44/50 samples detected ortho-phosphoric acid, 6/50 samples not detected any form of phosphate. The concentration of phosphate group in detected samples varied from 67.9 mg/kg to 2499 mg/kg.

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