免疫亲和柱法测定生湿面制品中T-2毒素含量

Determination of T-2 Toxin in Raw Wet Noodle Products by Immunoaffinity Column

建立一种高效液相色谱-荧光法(High performance liquid chromatography-fluorescence detection, HPLCFLD)测定生湿面制品中T-2毒素含量的方法。样品经振荡提取、免疫亲和柱净化、4-二甲基氨基吡啶(4-Dimethylaminopyridine, DMAP)溶液和1-氰酸蒽(1-Anthroyl Cyanide, 1-AC)溶液衍生后,通过HPLC分离,外标法定量。结果表明:T-2毒素在10~200 ng/mL质量浓度范围内与色谱峰面积呈良好的线性关系(r=0.999 9);在10.0,30.0和100.0μg/kg 3个加标水平下,平均回收率分别为73.4%, 83.0%和94.6%, RSD分别为5.6%, 4.0%和1.4%;方法检出限(RS/N=3)为10μg/kg,定量限(RS/N=10)为30μg/kg。该方法简单、快速、灵敏,为生湿面制品中T-2毒素的含量测定提供了一种可靠方法。

A method for determination of T-2 toxin in raw wet noodle products by HPLC-FLD was developed. The sample was extracted by oscillation, purified by immunoaffinity column, derivatived by DMAP and 1-AC, separated by HPLC, and quantified by external standard method. The results showed that the concentration of T-2 toxin was linear with chromatographic peak area in the range form 10 to 200 ng/mL. The linear correlation coefficients(r) were more than 0.999 9. At the spiking levels of 10.0, 30.0 and 100.0 μg/kg, the average recoveries were 73.4%, 83.0% and 94.6%, respectively, and the relative standard deviations were 5.6%, 4.0% and 1.4%, respectively. The detection limit(S/N=3) was 10 μg/kg, and the quantitative limit(S/N=10) was 30 μg/kg. This method was simple, rapid and sensitive, and it provided a reliable method for the determination of T-2 toxin in wet noodle products.