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高效液相色谱法检测粮油中黄曲霉毒素方法验证 被引量:5

Method validation on determination of aflatoxins in cereal and oil by high performance liquid chromatography
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摘要 该文报道验证同时检测粮食、植物油中黄曲霉毒素B_1、B_2、G_1和G_2的免疫亲和柱净化一柱后光化学衍生一高效液相色谱方法。样品经甲醇一水(体积比为70:30)提取,通过免疫亲和柱富集和净化,采用Cloversil C_(18)色谱柱(4.6 mm×150 mm,粒度5μm),以甲醇:水(50:50)溶液为流动相,柱后光化学衍生,利用荧光检测器检测,黄曲霉毒素B_1、B_2、G_1和G_2检出限分别为0.5μg、0.2μg、0.7μg和0.2μg/kg,标准曲线线性范围分别为:O.51~10.19 ng/mL、0.15~2.92 ng/mL、0.54~10.71 ng/mL、0.16~3.3 ng/mL;在稻谷、食用油样品中,平均加标回收率为70.3%~109.8%,相对标准偏差为1.4%~9.1%,说明回收率、精密度均可满足实际工作要求。 This paper verifies for the simultaneous determination of aflatoxins ( AFs ) B1, B2, G1 and G2 in cereals and oil by high performance liquid chromatography ( HPLC ) with fluorescence detection after immunoaffinity column clean-up and post-column derivatization, cereals and oil sample was extracted with methanol-water ( 70 : 30, v/v ). The extract was purified by immunoaffinity column and the aflatoxins were separated by reversed-phase HPLC, and quantified with fluorescence detection after photochemical derivatization. The separation was performed on a cloversil column (4.6mm i.d. × 150 mm, 5μm ) with a mobile phase consists of methanol-water ( 70/30, v/v ), quantified with fluorescence detection after photochemical derivatization .The limits of detection were 0.5 μg, 0.2 μg, 0.7 μg, 0.2 μg/kg for AFs B1, B2, G1 and G2. The calibration curves for AFs B1, B2, G1 and G2 were made in the concentration range : 0.51 - 10.19ng/mL, 0.15 -2.92 ng/mL, 0.54- 10.71ng/mL, 0.16-3.3ng/mL, the cereals and oil sample recoveries were from 70.3%- 109.8%, relative standard deviations were between 1.4 % and 9.1%.
出处 《粮食与油脂》 北大核心 2011年第11期36-38,共3页 Cereals & Oils
关键词 免疫亲和柱 高效液相色谱 黄曲霉毒素 immunoaffinity column high performance liquid chromatography ( HPLC ) aflatoxins
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