摘要
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B1、B2、G1和G2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 UltimateXB-C18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B1、B2、G1和G2线性范围在0.350.0μg/L之间,线性相关系数均大于0.999,B1、B2、G1和G2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2.043.87%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B1,B2,G1和G2的准确测定。
Objective To establish an immunoaffinity chromatography-high performance liquid chromatography(HPLC) fluorescence detector coupled with post-column photochemical derivatization method for determination of the aflatoxin B_1, B_2, G_1, and G_2 in food.Methods The sample was tested by HPLC with fluorescence detector after being homogenizer extracted from methanol-water(70:30, V:V), purified by immunoaffinity chromatography column of aggregated aflatoxin, separated by Welch Ultimate~XB-C_(18) HPLC column, eluted with a mobile phase consisting of methanol and waters(45:55, V:V) and derived from post column photochemical derivative reactor.The content of aflatoxin B_1, B_2, G_1, and G_2 in food was measured using peak area external standard method.Results The calibration curves showed a good linearity in each concentration range with correlation coefficient greater than 0.999 within linear range 0.3~50.0 μg/L.The limits of detection(LODs) were 0.15, 0.05, 0.15 and 0.05 μg/kg for the aflatoxins B_1, B_2, G_1, and G_2 in food, respectively.The recovery rate was within 80.7 %~92.6 % at 3 adding levels with the relative standard deviation(RSDs) of 2.04~3.87%.Conclusion This method is sensitive, accurate and precise, which is in accordance with technical standards of the aflatoxins detection.It is proper for routine detection of the aflatoxins B_1, B_2, G_1, and G_2 in food.
出处
《食品安全质量检测学报》
CAS
2015年第12期5017-5022,共6页
Journal of Food Safety and Quality
基金
科技型中小企业技术创新项目(13C26213302371)~~
关键词
黄曲霉毒素
食品
高效液相色谱法
柱后光化学衍生
aflatoxins
food
high performance liquid chromatography
post-column photochemical derivatization
