UPLC-光化学衍生法测定粮油中黄曲霉毒素

Determination of aflatoxin in cereals and oils by UPLC photochemical derivatization

建立了超高效液相色谱(ultra performance liquid chromatography, UPLC)-光化学衍生技术检测粮油产品中黄曲霉毒素B_(1)、B_(2)、G_(1)、G_(2)含量的方法。样品经甲醇水溶液提取,免疫亲和柱富集净化后,采用Agilent Eclipse Plus C色谱柱(3.0 mm×100 mm, 1.8μm)分离,以甲醇/水(体积比47∶53)为流动相等度洗脱,柱后光化学衍生,荧光检测器检测。结果表明:在优化条件下,4种黄曲霉毒素在8.6 min内完成色谱分析,在0.033~10.6 ng/mL范围内线性关系良好,相关系数均大于0.999,检出限范围0.005~0.03μg/kg,定量限范围0.02~0.1μg/kg;平均回收率83.2%~104.1%,RSD为1.1%~5.1%。方法操作简便,灵敏度高,重现性好,结果准确可靠,适用于粮油中黄曲霉毒素快速确证与精准检测。

A method for the determination of aflatoxin B_(1),B_(2),G_(1),G_(2) in cereals and oils by ultra performance liquid chromatography(UPLC) photochemical derivatization was established. The sample was extracted with methanol aqueous solution, enriched and purified by immunoaffinity column, and then used Agilent Eclipse Plus Cchromatographic column(3.0 mm×100 mm, 1.8 μm) separation, elution with methanol/water(volume ratio 47 ∶53) as flow equivalence, post column photochemical derivation, and detection with fluorescence detector. The results showed that the chromatographic analysis of 4 aflatoxins was completed within 8.6 min under the optimized conditions, the linearity was good within the range of 0.033-10.6 ng/mL, the correlation coefficient was greater than 0.999, and the detection limit was 0.005-0.03 μg/kg, limit of quantitation 0.02-0.1 μg/kg. The average recovery was 83.2 %-104.1 %, RSD was 1.1 %-5.1 %. The method was simple, sensitive, reproducible and accurate. It was suitable for rapid confirmation and accurate detection of aflatoxin in cereals and oils.