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目的建立免疫亲和柱净化-柱后光化学衍生-高效液相色谱-荧光法(HPLC-FLD),同时测定啤酒中黄曲霉毒素B_1、B_2、G_1、G_2。方法啤酒样品除尽二氧化碳后,氮吹至近干,用乙腈-水(20∶80,V/V)提取,提取液经免疫亲和柱净化,甲醇洗脱,洗脱液氮气吹干,溶剂换为乙腈-水(20∶80,V/V),上高效液相色谱,C_(18)柱分离,经光化学柱后衍生器衍生、荧光检测器检测,外标法定量。结果 4种黄曲霉毒素在相应的浓度范围内线性相关良好,相关系数(r)为0.999 2~0.999 5,检出限为0.01μg/kg~0.08μg/kg,加标回收率为90.55%~107.51%,加标回收实验的相对标准偏差(RSD)为0.47%~7.37%。结论该法灵敏度高、准确性好,可用于啤酒中4种黄曲霉毒素的测定。
OBJECTIVE To establish an HPLC-FLD method for the determination of aflatoxins B_1, B_2, G_1, G_2 in beer by immunoaffinity column cleanup-column photochemical derivatization-high performance liquid chromatography-fluorescence spectrometry. Methods After the beer sample was completely eliminated with carbon dioxide, the nitrogen was blown to near dryness and extracted with acetonitrile-water (20:80, V / V). The extract was purified by immunoaffinity column and eluted with methanol. (20:80, V / V), high performance liquid chromatography (HPLC), C 18 column separation, derivatization with photochemical post-column derivatization, fluorescence detector detection and external standard quantification. Results The four aflatoxins showed a good linear correlation in the corresponding concentration range with a correlation coefficient (r) of 0.999 2 to 0.999 5 and a detection limit of 0.01 μg / kg to 0.08 μg / kg with a spike recovery of 90.55% 107.51%. The relative standard deviations (RSDs) of spiked recovery experiments ranged from 0.47% to 7.37%. Conclusion The method has high sensitivity and good accuracy and can be used for the determination of four aflatoxins in beer.