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    三溴化吡啶衍生-发光二极管激发的荧光光谱法快速测定玉米粉中黄曲霉毒素B1的含量

    Rapid Determination of Aflatoxin B1 in Corn Meal by Light- Emitting Diode Excited Fluorescence Spectrometry after Pyridine Tribromide Derivatization

    • 摘要: 以发光二极管(LED)为激发光源,光纤光谱仪为检测设备,构建了LED激发的小型荧光光谱检测装置;利用三溴化吡啶衍生黄曲霉毒素B1(AFB1)产生强荧光信号,提出了快速测定玉米粉中AFB1含量的方法。称取5 g样品,加入25 mL 80%(体积分数)甲醇溶液和1.0 g氯化钠粉末,超声提取20 min,过滤。分取5 mL滤液,过C18固相萃取小柱,得到澄清透明溶液。分取2 mL,加入1 mL 200 mg·L-1三溴化吡啶溶液,于60 ℃恒温衍生反应4 min。在LED激发波长370 nm下,记录体系在429 nm处的荧光强度。结果表明:AFB1质量浓度在10~500 μg·L-1内与体系荧光强度呈线性关系,检出限(3s/k)为3.47 μg·L-1;对实际样品进行加标回收试验,AFB1回收率为80.1%~109%,测定值的相对标准偏差(n=5)为2.4%~7.7%。

       

      Abstract: A light-emitting diode (LED) excited micro fluorescence spectrum detection device was constructed with LED as the excitation light source and optical fiber spectrometer as the detection equipment. Aflatoxin B1 (AFB1) could produce strong fluorescence signal after pyridine tribromide derivation, and a method for the rapid determination of AFB1 in corn meal was proposed. The sample (5 g) was taken, and 25 mL of 80% (volume fraction) methanol solution and 1.0 g of sodium chloride powder were added. The mixture was extracted ultrasonically for 20 min and filtered, and an aliquot (5 mL) of the filtrate was taken and passed through C18 cartridge. An aliquot (2 mL) was taken, and 1 mL of 200 mg·L-1 pyridine tribromide solution was added, and the derivative reaction was conducted at 60 ℃ for 4 min. The fluorescence intensity of the system at 429 nm was recorded under the LED excitation wavelength of 370 nm. It was shown that linear relationship between mass concentration of AFB1 and fluorescence intensity of the system was kept in the range of 10-500 μg·L-1, with detection limit (3s/k) of 3.47 μg·L-1. Test for recovery was made on the actual sample, and the recoveries of AFB1 were in the range of 80.1%-109%, with RSDs (n=5) of the determined values ranged from 2.4% to 7.7%.

       

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