[关键词]
[摘要]
目的 建立高效液相色谱-光化学衍生-荧光检测法测定沉香药材中黄曲霉毒素B1、B2、G1、G2。方法 采用高效液相色谱法,通过免疫亲和柱提取和净化,荧光检测器检测。Agilent Zorbax Ecilpse Plus C18色谱柱(250 mm×4.6 mm,5μm);流动相:甲醇-水(45:55);体积流量:0.8 mL/min;柱温:30℃;进样盘温度:4℃;荧光激发波长为360 nm,发射波长为450 nm。结果 黄曲霉毒素B1、B2、G1、G2分别在9.3~74.4、3.0~24.0、9.3~74.4、3.5~28.0 pg线性关系良好,r均大于0.998 0;检测限分别为1.86、0.60、1.86、0.70 pg,定量限分别为7.44、2.40、7.44、2.80 pg。平均回收率分别为78%、92%、82%、99%,RSD值分别为4.4%、3.0%、4.3%、2.8%。结论 所建立的方法结果准确、重复性、稳定性均良好,可用于沉香药材中黄曲霉毒素的质量控制。
[Key word]
[Abstract]
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.
[中图分类号]
R985
[基金项目]
南通市市级科技计划(指导性)立项项目(YYZ17091)