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目的建立一种超高效液相色谱法测定花生油中4种黄曲霉毒素(B_1、B_2、G_1和G_2)含量的方法。方法花生油样品经甲醇-水提取后,静置2 min~3 min,过滤后稀释,用免疫亲和柱净化、浓缩。采用BEH C_(18)色谱柱(50 mm×2.1 mm,1.7μm),考察了不同流动相等度和梯度洗脱法,优化后的方法以甲醇-水溶液为流动相进行梯度洗脱,设定激发波长为360 nm、发射波长为450 nm进行检测。结果空白样品无干扰,4种黄曲霉毒素B_1、B_2、G_2在0.10μg/L~50.00μg/L,G_1在0.50μg/L~50.00μg/L时,线性关系良好,相关系数(r)均>0.999,最低检出限为0.04μg/kg~0.25μg/kg,相对标准偏差(RSD)为1.13%~8.82%,回收率为87.4%~104.6%。结论本方法简便、快速、准确,检出限低,干扰小,无需衍生,可用于粮油食品中黄曲霉毒素的检测。
Objective To establish a method for the determination of four aflatoxins (B_1, B_2, G_1 and G_2) in peanut oil by ultra performance liquid chromatography. Methods Peanut oil samples were extracted with methanol-water and allowed to stand for 2 min to 3 min. After filtration, the samples were diluted and purified by immunoaffinity column. BEH C_ (18) column (50 mm × 2.1 mm, 1.7 μm) was used to investigate the mobile phase equilibration and gradient elution. The optimized method was eluted with methanol-water as mobile phase and the excitation Wavelength of 360 nm, the emission wavelength of 450 nm for testing. Results The blank samples had no interference. The linearity of four aflatoxins B_1, B_2 and G_2 was from 0.10μg / L to 50.00μg / L and the G_1 was from 0.50μg / L to 50.00μg / L. The correlation coefficients > 0.999, and the detection limit was 0.04μg / kg ~ 0.25μg / kg. The relative standard deviations (RSDs) ranged from 1.13% to 8.82%. The recoveries ranged from 87.4% to 104.6%. Conclusion The method is simple, rapid, accurate, low detection limit, small interference, without derivative, can be used for the detection of aflatoxins in cereals and oils.