NGHIÊN CỨU PHƯƠNG PHÁP XÁC ĐỊNH ĐỒNG THỜI 4-METHYLIMIDAZOLE VÀ 2-ACETYL-4-TETRAHYDROXY-BUTYLIMIDAZOLE TRONG MÀU CARAMEL VÀ CÁC SẢN PHẨM BẰNG PHƯƠNG PHÁP SẮC KÝ LỎNG GHÉP NỐI KHỐI PHỔ=DETERMINATION OF 4-METHYLIMIDAZOLE AND 2-ACETYL-4-TETRAHYDROXY-BUTYLIMIDAZOLE IN CARAMEL COLOR AND PRODUCTS BY LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY

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Tác giả: Thị Huyền Trang Lưu, Phương Thảo Nguyễn, Trung Dũng Nguyễn, Thị Trang Vũ

Ngôn ngữ: vie

Ký hiệu phân loại:

Thông tin xuất bản: Journal of Science and Technique: Section on Physics and Chemical Engineering, 2024

Mô tả vật lý: tr.7

Bộ sưu tập: Metadata

ID: 483631

Thêm vào giỏ

Phát triển phương pháp xác định đồng thời 4-MEI và THI trong nền caramel và các sản phẩm chứa caramel bằng LC-MS/MS với nhiều ưu điểm đơn giản, độ chọn lọc và độ nhạy cao. Quá trình tách sắc ký sử dụng cột C18 (100 × 2,1 mm, 1,7 μm), pha động gồm amoniformat pH = 4 và acetonitril chứa 0,1% acid formic cùng chế độ rửa giải gradient. Chất phân tích được phát hiện trên hệ khối phổ hai lần MS/MS với nguồn ion hóa ESI+. Mẫu được làm sạch và làm giàu trên cột SPE MCX. Thẩm định phương pháp cho khoảng tuyến tính của 4-MEI trong khoảng 5,0 - 500 ppb, của THI trong khoảng 1,0 - 500 ppb
MDL của phương pháp là 0,30 μg/kg của THI và 1,5 μg/kg của 4-MEI
MQL là 1 μg/kg với THI và 5 μg/kg với 4-MEI, độ lặp lại với 4-MEI (2,9 - 9,1%), THI (3,5 - 9,4%)
độ tái lập đối với 4-MEI (2,9 - 11,8%), THI (4,8 - 11,5%)
độ thu hồi với 4-MEI (82,7 - 106,4%), THI (87,2 - 109,7%) đạt yêu cầu của AOAC. Ứng dụng phương pháp phân tích 24 sản phẩm trên thị trường (bao gồm caramel, đồ uống, gia vị và bánh ngọt) cho thấy hàm lượng 4-MEI và THI của các sản phẩm tiêu dùng đều nằm trong giới hạn cho phép, các mẫu caramel nguyên chất có hàm lượng THI vượt quá giới hạn cho phép.The simultaneous determination of 4-MEI and THI in caramel and products by LC-MS/MS was developed with several advantages of simplicity, selectivity, and high sensitivity. Chromatographic separation was performed using a C18 column (100 × 2.1 mm, 1.7 μm), with a mobile phase consisting of ammonium formate pH = 4 and acetonitrile containing 0.1% formic acid employing a gradient elution mode. The analytes were detected using an MS/MS double mass spectrometer with an ESI+ ionization source. Samples were cleaned and enriched on a SPE MCX column. Method validaion resulted in a linear range of 5.0 - 500 ppb for 4-MEI, and 1.0 - 500 for THI, with LODs of 0.30 g/kg for THI and 1.5 μg/kg for 4-MEI, and LOQs of 1 μg/kg for THI and 5 μg/kg for 4-MEI. Repeatability and reproducibility for 4-MEI ranged from 2.9% to 9.1% and 2.9% to 11.8%, respectively, and for THI from 3.5% to 9.4% and 4.8% to 11.5%, respectively. Recovery rates for with 4-MEI and THI met AOAC's requirements, ranging from 82.7% to 106.4% and 87.2% to 109.7%, respectively. Application of the analytical method for 24 market products, including caramel, beverages, condiments, and cakes, showed that the 4-MEI and THI concentrations in consumer products were within the permissible limits, while pure caramel samples exceeded the permissible limits for THI concentrations.

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