ĐỊNH LƯỢNG 5-HYDROXYMETHYLFURFURAL TRONG MẬT ONG BẰNG PHƯƠNG PHÁP SẮC KÝ LỎNG HIỆU NĂNG CAO (HPLC-DAD)=DETERMINATION OF 5-HYDROXYMETHYLFURFURAL IN HONEY BY HIGH PERFORMANCE CHROMATOGRAPHYL METHOD (HPLC-DAD)

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Tác giả: Dương Đình Chung, Nguyễn Văn Hòa, Nguyễn Hữu Khánh Quan, Trần Nguyễn An Sa, Nguyễn Thị Ngọc Yến

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Thông tin xuất bản: Tạp chí Khoa học Công nghệ và Thực phẩm (Tên mới: Tạp chí Khoa học Đại học Công Thương), 2018

Mô tả vật lý: tr.106

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ID: 487548

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In this research, high performance liquid chromatography coupled with photodiode array detector (HPLC-DAD) has been reported to quantify 5-hydroxymethyfurfural (HMF) compounds in honey. This method has been validated according to the Association of Official Analytical Chemists (AOAC) and the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) guidelines and shown to be specificity, precise, accurate, lower limit of detection (LOD) and lower limit of quantitation (LOQ). The separation was developed by selecting Gemini NX C18 (250 mm × 4.6 mm, 5 µm) column as stationary phase and acetonitril:H2O = 85:15 (v/v) as mobile phase, flow rate of mobile phase was maintained at 1 mL/min at room temperature throughout the experiment, injection volume 50 µL. Quantification was achieved with photodiod arrays (DAD) detection at 284 nm. A good linearity was observed in the concentration range of 2-100 µg/mL with a correlation coefficient (R2 = 0.9996). LOD and LOQ on the sample were 0.25 mg/mL and 0.75 mg/mL, respectively and the recovery of method from 87.3 to 105.8%. Results of analysis of HMF content in 12 samples of honey in the market valued from 47.8 to 522.5 mg/kg. However, the results revealed that 75% of the samples were failing to meet the Codex Alimentarius standards because HMF content in most of samples was above the limit of 80 mg/kg. Keywords: Hydroxymethylfurfural (HMF), honey, liquid chromatography (HPLC), determination, process validation.Trong nghiên cứu này, 5-hydroxymethyfurfural (HMF) được định lượng bằng phương pháp sắc ký lỏng hiệu năng cao với đầu dò diod array (HPLC-DAD). Phương pháp định lượng được xác định theo hướng dẫn của Hiệp hội các nhà hóa phân tích chính thống (AOAC) và Hội đồng quốc tế về sự phù hợp các yêu cầu kỹ thuật của dược phẩm dùng cho người (ICH) thể hiện được tính đặc hiệu, độ chính xác, độ đúng, giới hạn phát hiện (LOD) và giới hạn định lượng dưới (LOQ). Sự phân tách được thực hiện với cột Gemini NX RP-C18 (250 mm × 4,6 mm, 5 µm) làm pha tĩnh
2 dung môi là acetonitril:H2O = 85:15 (v/v) làm pha động
tốc độ dòng duy trì 1 mL/phút ở nhiệt độ phòng trong suốt thí nghiệm
thể tích tiêm mẫu 50 μL. Phát hiện bằng đầu dò diod array (DAD) ở bước sóng 284 nm. Khoảng tuyến tính nằm trong khoảng nồng độ 2-100 µg/mL với hệ số xác định R2 = 0,9996. Giới hạn phát hiện (LOD) và giới hạn định lượng (LOQ) lần lượt là 0,25 µg/mL, 0,75 µg/mL và tương ứng với độ phục hồi từ 87,3% đến 105,8%. Kết quả phân tích hàm lượng HMF trong 12 mẫu mật ong đang lưu hành trên thị trường có giá trị từ 47,8 đến 522,5 mg/kg. Tuy nhiên, kết quả kiểm tra có 75% trong 12 mẫu có hàm lượng HMF vượt mức cho phép theo tiêu chuẩn Codex Alimentarius (80 mg/kg).Từ khóa: Hydroxymethylfurfural (HMF), mật ong, sắc ký lỏng (HPLC), định lượng, thẩm định quy trình

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