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Phương pháp chiết xuất hỗ trợ bằng siêu âm kết hợp với vi chiết tản mát lỏng–lỏng (US-DLLME) — Một phương pháp nhanh mới để đo lường các chuyển hóa phthalate trong móng tay
Tóm tắt
Một phương pháp mới, nhanh chóng, thân thiện với môi trường dựa trên chiết xuất hỗ trợ bằng siêu âm kết hợp với vi chiết tản mát lỏng–lỏng (US-DLLME) đã được phát triển và tối ưu hóa để đánh giá nồng độ của bảy chuyển hóa phthalate (bao gồm mono(ethyl hexyl) phthalate (MEHP), mono(2-ethyl-5-hydroxyhexyl) phthalate (5-OH-MEHP), mono(2-ethyl-5-oxohexyl) phthalate (5-oxo-MEHP), mono-n-butyl phthalate (MnBP), mono-isobutyl phthalate (MiBP), monoethyl phthalate (MEP) và mono-benzyl phthalate (MBzP)) trong móng tay người bằng UPLC-MS/MS. Việc tối ưu hóa phương pháp US-DLLME được thực hiện thông qua thiết kế tổ hợp Taguchi (mảng L9). Nhiều tham số như dung môi chiết xuất, thể tích dung môi, thời gian chiết xuất, axit, nồng độ axit và thời gian xoay vòng đã được nghiên cứu. Các điều kiện chiết xuất tối ưu đạt được là 180 μL trichloroethylene (dung môi chiết xuất), 2 mL axit trifluoroacetic trong methanol (2 M), 2 giờ chiết xuất và 3 phút thời gian xoay vòng. Phương pháp tối ưu hóa có độ chính xác cao (6–17 %). Độ chính xác dao động từ 79 đến 108 % và giới hạn định lượng của phương pháp (LOQm) dưới 14 ng/g cho tất cả các hợp chất. Phương pháp US-DLLME được phát triển đã được áp dụng để xác định các chuyển hóa mục tiêu ở 10 cá nhân người Bỉ. Nồng độ của các chất phân tích đo được trong móng tay dao động giữa <12 và 7982 ng/g. MEHP, các đồng phân MBP và MEP là các chuyển hóa chính và được phát hiện trong tất cả các mẫu. Việc thu nhỏ kích thước (thể tích dung môi hữu cơ thấp), chi phí thấp, tốc độ và sự đơn giản là những lợi thế chính của phương pháp dựa trên US-DLLME này.
Từ khóa
#US-DLLME #chiết xuất hỗ trợ bằng siêu âm #phthalate #chuyển hóa trong móng tay #UPLC-MS/MSTài liệu tham khảo
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