USB电源供电表面增强拉曼基底快速制备装置的开发及其在农药残留检测中的应用  

Development of fast fabrication device for surface enhanced Raman spectroscopy substrate synthesis based on USB-power supply and its application for pesticide detection

作　　者：朱津毅 黄天雄 王甜 杜一平[2] 龚雪 彭洁 李炜 ZHU Jinyi;HUANG Tianxiong;WANG Tian;DU Yiping;CONG Xue;PENG Jie;LI Wei(China Tobacco Jiangsu Industrial Co.,Ltd.,Quality Management Department of Nanjing Cigarette Factory,Nanjing 210019,China;Shanghai Key Laboratory of Functional Materials Chemistry,School of Chemistry&Molecular Engineering,East China University of Science and Technology,Shanghai 200237,China;Technology Center,China Tobacco Jiangsu Industrial Co.,Ltd.,Nanjing 210019,China)

机构地区：[1]江苏中烟工业有限责任公司,南京卷烟厂品质管理处,南京210019 [2]上海功能性材料化学重点实验室,华东理工大学化学与分子工程学院,上海200237 [3]江苏中烟工业有限责任公司技术中心,南京210019

出　　处：《分析试验室》2024年第5期649-653,共5页Chinese Journal of Analysis Laboratory

基　　金：江苏中烟科技创新项目(202237)资助。

摘　　要：利用现用现制的方法快速制备SERS基底,以解决基底因储藏而导致稳定性变差和使用寿命不长的问题。研制了快速制备银溶胶基底的装置,该装置以USB电源供电,带有加热控温以及搅拌功能,可在10 min内制备银溶胶基底。透射电镜(TEM)结果显示,利用该装置制备的银溶胶纳米颗粒(AgNPs)分布均匀,粒径约80 nm;用于对罗丹明6G进行检测,多批次制备基底的SERS信号较强且稳定,相对标准偏差(RSD)在5%左右。将该装置用于检测苹果汁中农药残留敌草快,检出限达5.3μg/L,与气相色谱-质谱联用(GC-MS)和超高效液相色谱-质谱联用(UHPLC-MS)法的检出限结果相当;且1581 cm^(-1)处的SERS信号强度与敌草快浓度间具有良好的线性关系,相关系数(R^(2))为0.992,加标回收率在107%~112%之间,RSD在1.4%~3.6%之间。使用现制的银溶胶基底检测苹果汁中的敌草快残留灵敏度和准确度较高,为农残快速检测提供了一个新途径。A method for freshly synthesized surface enhanced Raman spectroscopy(SERS)substrate was proposed to solve the problem of low stability and short life of the substrate due to aggregation of nanoparticles.Based on USB power supply,a device with functions of heating,temperature control and stirring was designed and fabricated to synthesize silver colloid.Preparation of a substrate of Ag colloid for SERS detection could be completed in about 10 min by this device.The transmission electron microscope(TEM)image revealed that Ag nanoparticles(AgNPs)in the synthesized colloid show uniform distribution,with the particle size of about 80 nm.SERS signal of R6G was strong and stable,and the relative standard deviation(RSD)for five-batch substrates was around 5%.The limit of detection(LOD)of pesticide diquat in apple juice by SERS using the synthesized substrate was 5.3μg/L,closing to those obtained by gas chromatography-mass spectrometry(CC-MS)and ultrahigh performance liquid chromatography-mass spectrometry(UHPLC-MS)methods.Therewas a linear relationship between SERS signal intensity at 1581 cm^(-1)and concentration of diquat,and the correlation coefficient(R^(2))was 0.992.The recoveries were in the range of 107%-112%,and the relative standard deviations(RSDs)were 1.4%-3.6%.The sensitivity and accuracy of detecting diquat in apple juice by using the synthesized substrate were high,supplying a new way for the rapid detection of pesticide residuals.

关 键 词：表面增强拉曼光谱 基底 制备装置 农药 快检 

分 类 号：O657.3[理学—分析化学]