Nghiên cứu định lượng cynarin trong thực phẩm bảo vệ sức khỏe chứa actiso bằng phương pháp sắc ký lỏng hiệu năng cao=Study on determination of cynarin in dietary supplement containing artichoke by high performance liquid chromatography

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

Mô tả vật lý: tr.212-225

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ID: 481733

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Ở Việt Nam, cho đến nay chưa có công bố nào về việc tiêu chuẩn hóa và kiểm nghiệm cynarin trong thực phẩm, thực phẩm bảo vệ sức khỏe có chứa actiso. Do đó, để kiểm soát và đảm bảo chất lượng sản phẩm, nghiên cứu này đã phát triển phương pháp HPLC-PDA để định lượng cynarin trong thực phẩm bảo vệ sức khỏe chứa actiso. Mẫu được chiết lặp hai lần bằng hỗn hợp dung môi methanol: nước (80:20, v/v), siêu âm ở 50°C trong 20 phút. Dịch chiết được ly tâm với tốc độ 6000 vòng/phút trong 5 phút và lọc, tiêm vào hệ HPLC với cột XBridge C18 (250 mm × 4,6 mm, 5 µm) và tiền cột tương ứng. Pha động gồm hai dung môi acid phosphoric 0,1% và acetonitril rửa giải theo chương trình gradient, tốc độ dòng 1 mL/phút. Bước sóng phát hiện của cynarin là 322nm. Phương pháp cho khoảng tuyến tính 0,25 – 49,4 µg/mL (R2 = 1), giới hạn phát hiện và giới hạn định lượng lần lượt là 3,0 mg/kg và 10 mg/kg, độ thu hồi từ 86,5 – 109%, độ lặp lại (1,43 – 4,48%) đáp ứng yêu cầu AOAC. Phương pháp đã được áp dụng để phân tích hàm lượng cynarin trong 15 mẫu thực phẩm bảo vệ sức khỏe có actiso trên thị trường.There has been no announcement on the standardization and testing of cynarin in dietary supplements containing artichokes in Vietnam. The high-performance liquid chromatography (HPLC) method was developed to determine cynarin in dietary supplements containing artichokes. The sample was extracted twice with 80% methanol solvent and ultrasonicated at 50°C for 20 minutes. Centrifuge at 6000 rpm for 5 minutes, filter, and inject into HPLC system with XBridge C18 column (250 mm x 4,6 mm, 5 µm) and corresponding pre-column, mobile phase consisting of two solvents phosphoric acid 0,1% and acetonitrile eluted according to gradient program, flow rate 1mL/min, detection wavelength 322nm. The calibration curves for cynarin had R2 = 1, and the validation parameters met AOAC standards. The method detection limits and the limit of quantification were 3.00 mg/kg and 10.0 mg/kg, respectively. The validated method was applied to determine cynarin in 15 dietary supplement samples. The content of cynarin varied depending on the manufacturer.

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