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B_(1)(AFB_(1))产生强荧光信号,提出了快速测定玉米粉中AFB_(1)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C_(18)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:AFB_(1)质量浓度在10~500μg·L^(-1)内与体系荧光强度呈线性关系,检出限(3s/k)为3.47μg·L^(-1);对实际样品进行加标回收试验,AFB_(1)回收率为80.1%~109%,测定值的相对标准偏差(n=5)为2.4%~7.7%。
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 B_1(AFB_1) could produce strong fluorescence signal after pyridine tribromide derivation,and a method for the rapid determination of AFB_1 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 C_(18) 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 AFB_1 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 AFB_(1) were in the range of 80.1%-109%,with RSDs(n=5) of the determined values ranged from 2.4% to 7.7%.
作者
杨卓燃
李龙
吴琼
杜一平
YANG Zhuoran;LI Long;WU Qiong;DU Yiping(Shanghai Key Laboratory of Functional Materials Chemistry,School of Chemistry and Molecular Engineering,East China University of Science and Technology,Shanghai 200237,China;Institute of Chemistry,Henan Academy of Sciences,Zhengzhou 450002,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2023年第4期448-452,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
