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目的建立一种免疫亲和固相萃取柱净化-高效液相色谱柱后光化学衍生-荧光检测器同时测定食品中黄曲霉毒素B_1、B_2、G_1和G_2的方法。方法以甲醇-水(70:30,V:V)为提取溶剂,采用高速均质提取,并经过黄曲霉毒素免疫亲和柱净化。结果经月旭公司Welch Ultimate~XB-C_(18)色谱柱(250 mm×4.6 mm,5μm)分离后使用光化学衍生器进行柱后衍生,并采用带荧光检测器的高效液相色谱仪检测,流动相为甲醇/水(45:55,V:V)。黄曲霉毒素B_1、B_2、G_1和G_2线性范围在0.3~50.0μg/L之间,线性相关系数均大于0.999,B_1、B_2、G_1和G_2检出限分别为0.15μg/kg、0.05μg/kg、0.15μg/kg、0.05μg/kg。在3个加标浓度下大米、花生和瓜子等试样的回收率在80.7%~92.6%之间;相对标准偏差(RSD)在2.04~3.87%之间。结论该方法的灵敏度、准确度和精密度均符合黄曲霉毒素的检测技术要求,且简便快速,适用于食品中黄曲霉毒素B_1,B_2,G_1和G_2的准确测定。
OBJECTIVE To establish a method for the simultaneous determination of aflatoxins B 1, B 2, G 1 and G 2 in foodstuffs by immunoaffinity solid phase extraction (SPE) column chromatography and high performance liquid chromatography with photochemical derivatization - fluorescence detector. Methods The extraction solvent was methanol - water (70:30, V: V), extracted by high speed homogenization and purified by aflatoxin immunoaffinity column. Results After separation by Welch Ultimate ~ XB-C_ (18) column (250 mm × 4.6 mm, 5 μm), the column was derivatized with photochemical derivatization and detected by high performance liquid chromatography with fluorescence detector , The mobile phase was methanol / water (45:55, V: V). The linear correlation coefficients of aflatoxins B_1, B_2, G_1 and G_2 ranged from 0.3 to 50.0μg / L, and the linear correlation coefficients were all above 0.999. The detection limits of B_1, B_2, G_1 and G_2 were 0.15μg / kg and 0.05μg / kg , 0.15 μg / kg, 0.05 μg / kg. The recoveries of rice, peanut and melon seeds were between 80.7% and 92.6% at three spiked concentrations with relative standard deviations (RSDs) between 2.04-3.87%. Conclusion The sensitivity, accuracy and precision of this method are in accordance with the requirements of aflatoxin detection technology. The method is simple and rapid and is suitable for the accurate determination of aflatoxins B_1, B_2, G_1 and G_2 in food.