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CHI TIẾT
Nghiên cứu xây dựng quy trình phân tích triclosan và triclocarban trong một số dạng mỹ phẩm bằng HPLC
Development of an HPLC method for analysis of triclosan and triclocarban in cosmetic products
Võ Trần Ngọc Hùng, Lê Thị Hường Hoa, Thái Nguyễn Hùng Thu
Số: 518 - Tháng 6/2019 - Trang 21-25

Triclosan (TCS) có tác dụng ức chế sự phát triển vi khuẩn ở nồng độ thấp và có tác dụng tiêu diệt vi khuẩn ở nồng độ cao, ngoài ra nó còn có tác dụng với nhiều loại vi nấm nên thường được sử dụng với hai mục đích chính: Bảo quản sự ổn định của chế phẩm và tiệt khuẩn, khử trùng, tẩy uế. Triclocarban (TCC) cũng có tác dụng tương tự. Triclocarban khá nhạy cảm đối với vi khuẩn Gram (+). Theo Hiệp định hòa hợp ASEAN về quản lý mỹ phẩm nồng độ TCS tối đa cho phép trong nước súc miệng là 0,2 %, trong kem đánh răng và các sản phẩm vệ sinh cá nhân khác là 0,3 %. Nồng độ TCC tối đa được sử dụng với mục đích bảo quản là 0,2 % tuy nhiên nồng độ được sử dụng trong các sản phẩm rửa sạch (rinse-off products) có thể lên đến 1,5 %.

Việc lạm dụng TCS và TCC đã không những làm gia tăng khả năng đề kháng của vi khuẩn với TCS và TCC mà còn làm gia tăng đề kháng của vi khuẩn với một số loại kháng sinh. Do vậy, việc sử dụng TCS và TCC trong các chế phẩm cần được tuân thủ một cách nghiêm ngặt hơn. Nghiên cứu này nhằm xây dựng phương pháp cho phép xác định đồng thời hàm lượng TCS và TCC trong một số dạng mỹ phẩm là kem đánh răng và nước rửa tay.

            Nguyên liệu

            Chất đối chiếu: Triclosan (lô 106MHC CAS 3380-34-5, Anh), hàm lượng 99,0 %; Triclocarban (lô MKBT7249V CAS 101-20-2, Hoa Kỳ), hàm lượng 99,0 %.

Phương pháp nghiên cứu

            - Khảo sát điều kiện xử lý mẫu: Chọn dung môi và phương pháp chiết sao cho chiết được hoàn toàn chất phân tích từ nền mẫu, loại bỏ tối đa ảnh hưởng của nền mẫu dựa vào 3 yếu tố chính: tính tan của chất phân tích, đặc điểm nền mẫu, phương pháp phân tích.

            - Khảo sát khả năng phân tích đồng thời TCS và TCC và xác định điều kiện sắc ký.

            - Thẩm định các phương pháp đã chọn về: Độ đặc hiệu, khoảng tuyến tính, độ lặp lại, độ chính xác trung gian, độ đúng, giới hạn phát hiện và giới hạn định lượng, khoảng xác định của phương pháp.

- Các kết quả thực nghiệm được tính toán và xử lý thống kê trên Microsoft Excel với các hàm thống kê thông dụng.

Kết luận

   Một quy trình cho phép phân tích đồng thời triclosal và triclocarban trong kem đánh răng và nước rửa tay bằng HPLC có quá trình xử lý mẫu đơn giản bằng chiết siêu âm với acetonitril rồi thêm nước theo tỷ lệ 7:3 đã được thiết lập. Kết quả thẩm định tại giới hạn định lượng cho thấy với điều kiện phân tích này phương pháp có độ lặp lại cao, độ đúng tốt, khoảng tuyến tính đủ rộng và có giới hạn phát hiện tốt. Đã áp dụng phương pháp để phân tích 13 mẫu kem đánh răng và 7 mẫu nước rửa tay trên thị trường, các mẫu có chứa TCS, TCC đều ở mức cho phép. Hy vọng quy trình này có thể triển khai áp dụng được tại các đơn vị kiểm nghiệm mỹ phẩm.

An HPLC method was proposed for simultaneous analysis of triclosan (TCS) and triclocarban (TCC) in cosmetics, tooth-pastes and hand washes. TCS and TCC were extracted with a mixtrure of acetonitrile and water (70:30) in the concentration of 1.5 to 4.5 µg/ml. For injection, the obtained extracts were cleaned by passing through a filter membrance with pore size of 0.45µm. The HPLC procedure was as follows: Column - Octylsilyl Silica gel C8 (250 × 4.6 mm; 5µm), temperature - 40 oC; Detector - UV (288 nm); Mobile phase - mixture of acetonitrile and water (70:30); Flow rate - 1.0 ml/min.; Injection volume was 20 µl. The method was validated for the specificity, linear range, precision, accuracy, LOD, LOQ, proving suitable for determination of triclosan and triclocarban in the hand wash and tooth-paste commodies, and also, very time-saving (only 30 minutes for a run). Experimentally, 13 cosmetic tooth-paste and 07 hand wash samples were analysed. Of these, TCS was detected in 01 tooth-paste and 04 hand wash samples, and TCC in 03 hand wash samples. Practically, the method proved applicable to detection of TCC and TCS in products of the kind, as now they have had no acceptable authorized limits formerly recorded in the Asean Cosmetic Annex.

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