Xây dựng quy trình định lượng đồng thời đồng phân cefpodoxim proxetil trong viên nén bằng phương pháp HPLC với đầu dò PDA

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Tác giả: Thị Bảo Ngọc Phạm, Thị Phương Anh Trần, Quốc Kỳ Trương

Ngôn ngữ: vie

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Thông tin xuất bản: Tạp chí Y Dược học Phạm Ngọc Thạch, 2024

Mô tả vật lý: tr.187

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ID: 479438

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Mục tiêu: Nghiên cứu này nhằm đưa ra phương pháp định lượng đồng thời các đồng phân của cefpodoxim proxetil trong viên nén bằng phương pháp HPLC với đầu dò PDA. Đối tượng và phương pháp nghiên cứu: Đối tượng của nghiên cứu này là viên nén có chứa hoạt chất cefpodoxim proxetil dưới dạng hỗn hợp đồng phân. Đồng phân R của cefpodoxim proxetil đã được điều chế và kiểm tra độ tinh khiết theo chuyên luận USP 44. Điều kiện sắc ký đã được khảo sát và tối ưu hóa bằng phần mềm Design Expert sử dụng mô hình thiết kế CCD với hai yếu tố bao gồm nhiệt độ cột và tỷ lệ methanol trong pha động. Phương pháp này đã được thẩm định theo ICH Q2 (R1) và “Sổ tay hướng dẫn đăng ký thuốc” của Bộ Y tế. Kết quả: Phương pháp HPLC-PDA đã được phát triển thành công để định lượng các đồng phân của cefpodoxim proxetil trong viên nén. Các điều kiện sắc ký tối ưu được liệt kê như sau: cột Sunfire C18 (150 x 4,6 mm
5 µm), nhiệt độ cột 33˚C với pha động là hỗn hợp methanol-nước (51:49, tt/tt), tốc độ dòng 1 ml/phút và bước sóng phát hiện là 235 nm. Phương pháp đạt tính tuyến tính trong khoảng nồng độ 25-250 µg/ml đối với cả hai đồng phân. Độ đúng của đồng phân R trong khoảng từ 100,74-102,71% và đồng phân S trong khoảng từ 100,25-101,48%. Độ lặp lại của đồng phân R và đồng phân S có RSD lần lượt là 1,62%, 1,54% và độ chính xác trung gian của đồng phân R và đồng phân S có RSD lần lượt là 1,24%, 1,14%. Kết luận: Đề tài này đã xây dựng thành công quy trình định lượng đồng thời viên nén cefpodoxim proxetil bằng phương pháp HPLC-PDA. Quy trình này đạt các chỉ tiêu thẩm định, có tính chọn lọc, độ đúng và độ chính xác cao. Abstract Objectives: This research aimed to quantify cefpodoxime proxetil (CFP) epimers in tablets by HPLC-PDA. Methods: The subject of this study was cefpodoxime proxetil tablets in the form of an epimers mixture. Cefpodoxime proxetil epimers were quantified by HPLC with a PDA detector, while the R-isomer of cefpodoxime proxetil was prepared and tested for purity according to USP 44 monograph. The chromatographic condition was optimized by the Design Expert program using central composite design (CCD) with two factors: column temperature and mobile phase ratio. The developed method was validated according to ICH Q2 (R1) and the “Handbook for Drug Registration” of the Ministry of Health. Results: An HPLC-PDA method was successfully developed to quantify cefpodoxime proxetil epimers in tablets. The optimal chromatographic conditions were listed as follows: the Sunfire C18 (150 x 4.6 mm
5 µm) column was set at 33˚C, the mobile phase was the mixture of solvent methanol-water (51:49, v/v), the flow rate of 1 ml per minute, and the detection wavelength was 235 nm. The method was validated over the concentration range of 25-250 µg/ml for both epimers. The accuracy of R-epimer ranged between 100.74 to 101.71%, and S- epimer ranged between 100.25 to 101.48%. The intra-day precision varied 1.62% for R- epimer and 1.54% for S- epimer and the inter-day precision varied 1.24% for R- epimer and 1.14% for S- epimer. Conclusion: This study has developed a process to simultaneously quantify cefpodoxime proxetil tablets using the HPLC-PDA method. This method was validated, and has high selectivity, precision, and accuracy. DOI: 10.59715/pntjmp.3.3.21

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