氧化锌纳米棒光电极对核黄素的光致电化学响应及应用

doi:10.7503/cjcu20160522

高等学校化学学报 ›› 2016, Vol. 37 ›› Issue (12): 2144.doi: 10.7503/cjcu20160522

氧化锌纳米棒光电极对核黄素的光致电化学响应及应用

何艳艳¹, 葛军营^1,², 赵常志¹()

1. 生化分析山东省重点实验室, 青岛科技大学化学与分子工程学院, 青岛 266042
2. 潍坊工程职业学院应用化学与生物工程学院, 青州 262500

收稿日期:2016-07-19 出版日期:2016-12-10 发布日期:2016-11-15
作者简介:联系人简介: 赵常志, 男, 博士, 教授, 主要从事光电化学和电分析化学方面的研究. E-mail:zhaocz@qust.edu.cn
基金资助:
国家自然科学基金(批准号: 21475072)、肿瘤标志物传感分析教育部重点实验室开放基金(批准号: SATM201503)和电分析化学国家重点实验室开放基金(批准号: SKLEAC201106)资助

Photoelectrochemical Response and Application of ZnO Nanorods Photoelectrode to Riboflavin^†

HE Yanyan¹, GE Junying^1,², ZHAO Changzhi^1,^*()

1. Shandong Provincial Key Laboratory of Biochemical Analysis, College of Chemistry & Molecular Engineering,Qingdao University of Science & Technology, Qingdao 266042, China
2. Institute of Applied Chemistry& Biological Engineering, Weifang Engineering Vocational College, Qingzhou 262500, China

Received:2016-07-19 Online:2016-12-10 Published:2016-11-15
Contact: ZHAO Changzhi E-mail:zhaocz@qust.edu.cn
Supported by:
† Support by the National Natural Science Foundation of China(No.21475072), the Open-end Fund of Key Laboratory of Sensor Analysis of Tumor Marker of Ministry of Education, China(No.SATM201503) and the Open-end Fund of State Key Laboratory of Electroanalytical Chemistry, China(No.SKLEAC201106)

摘要/Abstract

摘要：

基于核黄素在第二工作电极上的预还原, 将还原型核黄素作为电子给体纳入氧化锌纳米棒光电极的光致电化学反应过程, 构建了一种新的光致电化学反应系统. 优化了电化学制备氧化锌纳米棒光电极的方法, 研究了核黄素与氧化锌纳米棒光电极的光致电化学反应机理, 建立了一种测定核黄素的光致电化学分析法. 在pH=6.5的缓冲溶液中, 以玻碳电极为预还原电极, 在峰值波长为365 nm、能量为450 μW/cm²的光照下, 在偏压0.1 V处测得的光电流与1.00×10^-5~1.00 μmol/L核黄素浓度的对数值成正比, 检出限为6.0×10^-7 μmol/L(S/N=3), 灵敏度为195.6 nA/lg[c(μmol/L)]. 对实际样品测定的相对标准偏差小于6.25%, 回收率为99.0%~104%, 常见生化物质对核黄素光电流的响应无干扰.

关键词: 核黄素, 氧化锌纳米棒, 光致电化学分析法, 四电极电化学系统

Abstract:

In this work, based on the pre-reduction of riboflavin(RF) on the second working electrode, a new photoelectrochemical(PEC) system was fabricated by the reduced RF as an electron donor incorporated into PEC reaction process of zinc oxide nanorods photoelectrode(ZnONRP). After optimizing the electro-chemical preparation for ZnONRP and studying the reaction mechanism of RF with ZnONRP, a PEC method for the determination of RF was developed. Under the optimized conditions of pH=6.5, -0.40 V as pre-reduction potential, illumination at 365 nm and light energy of 450 μW/cm², the photocurrent at bias voltage 0.1 V is proportional to the logarithm of RF concentration in the range of 1.00×10^-5—1.00 μmol/L with sensitivity of 195.6 nA/lg[c(μmol/L)], and the detection limit was estimated to be 6.00×10^-7 μmol/L(S/N=3). Determination results for real samples showed that the relative standard deviation is less than 6.25% and the recovery rate is 99.0%—104%. Compared with other methods for the determination of RF, the proposed method has various advantages, such as wide measurement range, high sensitivity, simple equipment and convenient operation. And common biochemical substances were not interfering with the photocurrent response of RF.

Key words: Riboflavin, ZnO nanorods, Photoelectronchemical analysis, Four-electrode electrochemical system

中图分类号:

O657.1

TrendMD:

何艳艳, 葛军营, 赵常志. 氧化锌纳米棒光电极对核黄素的光致电化学响应及应用. 高等学校化学学报, 2016, 37(12): 2144.

HE Yanyan, GE Junying, ZHAO Changzhi. Photoelectrochemical Response and Application of ZnO Nanorods Photoelectrode to Riboflavin^†. Chem. J. Chinese Universities, 2016, 37(12): 2144.

图/表 9

Fig.1 SEM image of the cross-section of ZnONRPInset is the surface photography of ZnONRP.

Fig.2 SEM image of the cross-section of ITO electrode

Fig.3 XRD pattern of ZnONRP surface

Fig.4 Cyclic voltammograms of RF solution(1.00×10-4 mol/L) before(a) and after electrochemical reduction(b)Inset is the structural formula of RF.

Fig.5 Fluorescence spectra of RF solution(1.00×10-6 mol/L) before(a) and after electrochemical reduction(b)

Fig.6 Photoelectrochemical response mechanism of RF on ZnONRP(A) and photocurrent responses(B) of blank solution(a), the unreduced RF(b) and reduced RF(c) on ZnONRP

Fig.7 Photocurrent responses to various concentration of RFs(A) and response curve(B)(A) From left to right, cRF/(μmol·L-1): 0, 1.00×10-5, 1.00×10-4, 1.00×10-3, 1.00×10-2, 0.10, 0.50, 1.00. (B) Inset is the calibration curve on the photocurrent responses to concentration logarithm.

Fig.8 Reduction current curve of RF at GCE(a) and photocurrent response curve of RF at ZnONRP(b)

Table 1 Determination results of the riboflavin in millet

Sample	Found/(μg·g^-1)	RSD(%)	Fluorescence/(μg·g^-1)	Added(μg·g^-1)	Total/(μg·g^-1)	Recovery(%)
1	1.92	5.48	1.85	2.00	4.06	104
2	1.38	6.25	1.42	1.50	2.85	99.0
3	1.26	5.76	1.32	1.00	2.29	101

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氧化锌纳米棒光电极对核黄素的光致电化学响应及应用

Photoelectrochemical Response and Application of ZnO Nanorods Photoelectrode to Riboflavin^†

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氧化锌纳米棒光电极对核黄素的光致电化学响应及应用

Photoelectrochemical Response and Application of ZnO Nanorods Photoelectrode to Riboflavin†

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Photoelectrochemical Response and Application of ZnO Nanorods Photoelectrode to Riboflavin^†