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比较了牛奶中黄曲霉毒素测定的3种液相色谱分析方法。样品经直接稀释、免疫亲和柱净化,以乙腈-甲醇-水体积比(22︰22︰46)为流动相,分别经柱后光化学衍生化、未衍生化及碘衍生化-液相色谱-荧光法进行测定。柱后光化学衍生化,黄曲霉毒素M_2,M_1线性范围为0.02~20μg/L,G_2,B_2 0.005~20μg/L,G_1,B_1 0.01~20μg/L,相关系数≥0.999,定量限为0.000 5~0.002μg/kg,加标回收率79%~116%;柱后碘衍生化,M_2,M_1线性范围分别为0.02~20,0.05~20μg/L,其余4种均为0.01~20μg/L,相关系数≥0.999,定量限0.001~0.005μg/kg,回收率74~121%;未经衍生化直接进样,G_2,B_2线性范围0.005~20μg/L,其余4种为0.02~20μg/L,相关系数≥0.998,定量限0.000 5~0.003μg/kg,回收率82%~121%。结果表明,柱后光化学衍生测定6种黄曲霉毒素在线性范围、灵敏度和定量限等方面均具有优势。
Three methods of liquid chromatography for the determination of aflatoxins in milk were compared. The samples were directly diluted and purified with immunoaffinity column. The mobile phase was acetonitrile - methanol - water (22:22:46), and the derivatized, underivatized and iodinated derivatized LC - Fluorescence assay. Post-column photochemical derivatization showed that the linear range of aflatoxins M_2 and M_1 was 0.02 ~ 20μg / L, G_2 and B_2 were 0.005 ~ 20μg / L, G_1 and B_1 were 0.01 ~ 20μg / L with correlation coefficients ≥0.999. 0.002 μg / kg, and the recoveries were in the range of 79% -116%. The post-column iodine derivatization showed that the linear ranges of M_2 and M_1 were 0.02-20 and 0.05-20 μg / L, respectively, and the other four were 0.01-20 μg / L The linear range of G_2 and B_2 was 0.005 ~ 20μg / L, the other four were 0.02 ~ 20μg / L, the correlation coefficient was 0.999, the limit of quantification was 0.001 ~ 0.005μg / kg and the recovery was 74 ~ 121% The coefficient ≥0.998, the limit of quantification 0.000 5 ~ 0.003μg / kg, the recovery rate 82% ~ 121%. The results showed that post-column photochemical derivatization was superior to the six aflatoxins in terms of linear range, sensitivity and limit of quantification.