目的 建立高效液相色譜-光化學(xué)衍生-熒光檢測(cè)法測(cè)定沉香藥材中黃曲霉毒素B₁、B₂、G₁、G₂。方法 采用高效液相色譜法，通過免疫親和柱提取和凈化，熒光檢測(cè)器檢測(cè)。Agilent Zorbax Ecilpse Plus C₁₈色譜柱（250 mm×4.6 mm，5μm）；流動(dòng)相：甲醇-水（45：55）；體積流量：0.8 mL/min；柱溫：30℃；進(jìn)樣盤溫度：4℃；熒光激發(fā)波長(zhǎng)為360 nm，發(fā)射波長(zhǎng)為450 nm。結(jié)果 黃曲霉毒素B₁、B₂、G₁、G₂分別在9.3~74.4、3.0~24.0、9.3~74.4、3.5~28.0 pg線性關(guān)系良好，r均大于0.998 0；檢測(cè)限分別為1.86、0.60、1.86、0.70 pg，定量限分別為7.44、2.40、7.44、2.80 pg。平均回收率分別為78%、92%、82%、99%，RSD值分別為4.4%、3.0%、4.3%、2.8%。結(jié)論 所建立的方法結(jié)果準(zhǔn)確、重復(fù)性、穩(wěn)定性均良好，可用于沉香藥材中黃曲霉毒素的質(zhì)量控制。

Objective To establish an HPLC-florescence detection method for determination of aflatoxin B₁, B₂, G₁, and G₂ in Aquilariae Lignum Resinatum. Methods HPLC method was adopted, extracting and purifying were used with an immunoaffinity column, enhanced by a photochemical high-performance liquid chromatography, and detected by a fluorescent detector. The contents of aflatoxins were determined on Agilent C₁₈ column (250 mm×4.6 mm, 5 μm). The mobile phase was methanol-water (45:55) with a flow rate of 0.8 mL/min, and the column temperature was 30℃. The Sample tray temperature was 4℃. The excitation wavelength was set as 360 nm and the emission wavelength was 450 nm. Results Aflatoxins B₁, B₂, G₁, and G₂ had good linear relationship in the range of 9.3-74.4, 3.0-24.0, 9.3-74.4, and 3.5-28.0 pg with r values above 0.998 0. The average recovery rates were 78%, 92%, 82%, and 99% with the RSDs were 4.4%, 3.0%, 4.3%, and 2.8%, respectively. The detection limits of aflatoxins B₁, B₂, G₁, and G₂ were 1.86, 0.60, 1.86, and 0.70 pg, and the quantitative limits were 7.44, 2.40, 7.44, and 2.80 pg. respectively. Conclusion The method is accurate, reproducible, and stable, and can be used for the quality control of aflatoxins in Aquilariae Lignum Resinatum.

R985

南通市市級(jí)科技計(jì)劃（指導(dǎo)性）立項(xiàng)項(xiàng)目（YYZ17091）