Ứng dụng kỹ thuật LC-MS/MS để xác định chất cấm Cyproheptadin trong thực phẩm chức năng

0 Người đánh giá. Xếp hạng trung bình 0

Tác giả: Công Khánh Cao, Thị Thanh Hoa Mạc, Ngọc Diệp Nguyễn, Quang Hùng Nguyễn, Thị Vân Anh Nguyễn, Thị Thanh An Vũ

Ngôn ngữ: vie

Ký hiệu phân loại: 543.4 Electrochemical analysis

Thông tin xuất bản: Kiểm nghiệm và an toàn thực phẩm, 2023

Mô tả vật lý: 351-367

Bộ sưu tập: Metadata

ID: 502457

Thêm vào giỏ

Cyproheptadin (CYP) là một kháng histamin H1 thường bị trộn trái phép trong các thực phẩm chức năng để kích thích sự thèm ăn, tăng cân của trẻ nhỏ, hiện đã bị cấm sử dụng trong thực phẩm bảo vệ sức khỏe theo quy định tại Thông tư 10/2021-BYT. Phương pháp được nghiên cứu sử dụng hệ thống sắc ký lỏng khối phổ hai lần của Agilent Triple Quadrupole 6460 với mảnh 288,1 → 96,1 và 288,1 → 191,2 được lựa chọn để định lượng và định tính. Cột sắc ký XBridge C18 (100 mm × 2,1 mm, 3,5 μm) với pha động gồm acetonitril và acid formic 0,1% được lựa chọn cho phép tách sắc ký. Chất phân tích được chiết bằng methanol và làm sạch bằng hỗn hợp bột PSA (Primary Secondary Amine) và bột C18. Độ thu hồi đạt trong khoảng 80 - 110% và độ đúng của phương pháp đạt yêu cầu về thẩm định phương pháp theo quy định của Hiệp hội các nhà hóa học phân tích chính thống (AOAC) ở các mức nồng độ thêm chuẩn trên ba nền mẫu thực phẩm bảo vệ sức khỏe dạng cốm, dạng siro và thực phẩm bổ sung dạng sữa bột. Giới hạn phát hiện và định lượng đạt được 0,08 mg/kg và 0,25 mg/kg với nền mẫu siro
0,15 mg/kg và 0,50 mg/kg với nền mẫu cốm và nền sữa bột. Phương pháp đã được áp dụng để phân tích 30 mẫu thực phẩm chức năng trên thị trường và phát hiện 01 mẫu siro dương tính (hàm lượng 1,67 mg/liều dùng 10 mL). Phương pháp có thể ứng dụng phương pháp để phân tích CYP trong các mẫu thực phẩm chức năng trên thị trường cũng như phát triển để phân tích đồng thời các chất trộn trái phép khác có tính chất và tác dụng tương tự trong các nghiên cứu tiếp theo.Cyproheptadine is an H1 antihistamine, that is often illegally added in dietary supplements to stimulate appetite and gain weight in children, currently banned for use in health supplements according to the provisions of Circular 10/2021-BYT. The method was using the Agilent Triple Quadrupole 6460 with fragments 288.1 → 96.1 and 288.1 → 191.2 selected for quantitative and qualitative. The separation was carried out on XBridge C18 column (100 mm × 2.1 mm, 3.5 μm) with a mobile phase consisting of acetonitrile and 0,1% formic acid. The analyte was extracted with methanol and cleaned up by d-SPE technique using a mixture of PSA and C18 powder. The recovery was in the range of 80-110%, the accuracy met the requirements of AOAC for method validation at spiked concentrations on three matrices of dietary supplements (granules, syrup, and powdered milk). Limits of detection and quantification were achieved at 0.08 mg/kg and 0.25 mg/kg with the syrup
0.15 mg/kg and 0.50 mg/kg with granule and powdered milk samples. The method has been applied to analyze 30 samples and detected cyproheptadine in a syrup sample at 1.67 mg/dose of 10 mL. This method can be applied to analyzing cyproheptadine in dietary supplements on the market as well as developing for simultaneous determination of other adulterants with similar properties and effects in our next studies.

1. Đọc trực tuyến

1. Đọc trực tuyến

Tạo bộ sưu tập với mã QR