论文部分内容阅读
目的建立高效液相色谱等浓度流动相同时测定黄曲霉毒素G_1、B_1、G_2、B_2的方法。方法样品经乙腈+水(84+16)溶解,用多功能振荡器超声提取30 min,多功能固相萃取柱净化,将净化液收集于10 ml比色管中,取少量净化液于10 ml一次性离心杯中,60℃水浴氮气吹至近干,用正己烷和三氟乙酸在40℃培养箱内衍生15 min,室温干燥,用乙腈+甲醇+水(22+22+56)溶解,过0.22μm小滤膜于样品瓶中,荧光检测器,流动相乙腈+甲醇+水(22+22+56)测定。结果黄曲霉毒素G_1、B_1、G_2、B_2分离效果好,回收率在83.7%~96.5%之间,RSD值在0.92%~2.74%之间,线性关系r=0.9 991~0.9 993,检出限分别为:0.050μg/kg,0.025μg/kg,0.100μg/kg,0.030μg/kg。结论高效液相色谱法优化测定食品中黄曲霉毒素灵敏度好,色谱条件比GB/T 5009.23-2006的梯度洗脱简单,快速,定量准确。
Objective To establish a method for simultaneous determination of aflatoxins G_1, B_1, G_2 and B_2 at the same concentration of mobile phase by high performance liquid chromatography. Methods The samples were dissolved in acetonitrile + water (84 + 16), extracted with a multi-functional oscillator for 30 min and cleaned up with a multi-functional solid-phase extraction cartridge. The purified solution was collected in a 10 ml cuvette. Disposable centrifuge cup, 60 ℃ water bath nitrogen to near dry, with hexane and trifluoroacetic acid in 40 ℃ incubator derived 15 min, at room temperature, with acetonitrile + methanol + water (22 +22 +56) dissolved, too 0.22μm small membrane in the vial, fluorescence detector, mobile phase acetonitrile + methanol + water (22 +22 +56) determination. Results The aflatoxins G_1, B_1, G_2 and B_2 had good separation efficiency and the recoveries ranged from 83.7% to 96.5%. The RSD values ranged from 0.92% to 2.74%. The linear relationship was 0.9991 ~ 0.9993. The detection limits Respectively: 0.050μg / kg, 0.025μg / kg, 0.100μg / kg, 0.030μg / kg. Conclusion The method of HPLC for the determination of aflatoxin in food has good sensitivity. The chromatographic conditions are simpler, faster and more accurate than the gradient of GB / T 5009.23-2006.