| 基于Au NPs@NU-901电化学传感器检测饼干中丁基羟基茴香醚的研究 |
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| 基金项目:广东省食品安全重点领域研发计划项目(2019B020211001)；国家重点研发计划项目课题项目(2019YFC1606101)；国家自然科学基金项目(21976213，21775167);中山大学大学生创新训练计划项目(20211283) |
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| 中文摘要:基于金属有机骨架的拓扑三维结构的高比表面积以及金纳米颗粒(Au NPS)的优异电催化活性，金纳米颗粒与金属有机框架的复合材料在电化学传感领域拥有应用潜力。该文成功合成了Au NPs@NU-901复合材料,并采用透射电镜、X射线衍射、红外光谱以及X射线光电子能谱对其进行表征。采用线性扫描伏安法和差分脉冲伏安法研究了复合材料对丁基羟基茴香醚(BHA)电化学氧化反应的催化能力。结果表明，Au NPs@NU-901对BHA的电化学氧化具有较好的催化能力。基于Au NPs@NU-901制备电化学传感器用于BHA的定量检测，BHA的氧化峰电流与其浓度在0.10~50 μmol/L范围内呈现良好线性关系，相关系数(r2)为0.994 8，检出限(S/N=3)为0.049 μmol/L，相对标准偏差(RSD)为3.6%。将该传感器应用于饼干样品中BHA的检测，加标回收率为95.6%~104%，样品检测结果与高效液相色谱法的测定结果吻合。方法的选择性好、灵敏准确，适合于饼干中BHA的检测。 |
| 中文关键词:金属有机框架 金纳米粒子(Au NPs) 电化学传感器 丁基羟基茴香醚 饼干 |
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| Determination of Butylated Hydroxyanisole in Biscuit Using an Electrochemical Sensor Based on Au Nanoparticles@NU-901 |
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| Abstract:Metal organic frameworks(MOFs) are characterized with high specific surface areas which are beneficial to adsorption,while Au nanoparticles(Au NPs) are known to have excellent catalytic activity.Therefore,the composites of Au NPs and MOFs have a wide application in electrochemical sensing.In this work,the composites of Au NPs@NU-901 were prepared and characterized by transmission electron microscopy,X-ray diffraction,infrared spectroscopy and X-ray photoelectron spectroscopy.The results obtained testified the successful synthesis of Au NPs@NU-901.The electrochemical performance of Au NPs@NU-901/GCE toward the electrocatalytic oxidation of butylated hydroxyanisole(BHA) was investigated by linear sweep voltammetry(LSV) and differential pulse voltammetry(DPV).The experimental results showed that Au NPs@NU-901/GCE could catalyze the electrochemical oxidation-reduction reaction of BHA,and the signal was enhanced more greatly compared with those of bare/GCE,NU-901/GCE and Au NPs/GCE.In addition,the oxidation mechanism of BHA was investigated by LSV.By exploring the relationship between peak potential and pH values ranging from 2.2 to 8.0,as well as the relationship among peak potential and peak currents and scanning rates ranging from 50 mV/s to 250 mV/s,it was proved that the oxidation-reduction reaction of BHA on Au NPs@NU-901/GCE exhibited a process involving two electrons and two protons.In order to improve the detection sensitivity,the conditions,including supporting electrolyte,drop-coating volume,accumulation potential and accumulation time,were optimized.Under the optimal conditions,an electrochemical sensor based on Au NPs@NU-901 was fabricated for the determination of BHA with a linear range of 0.10-50 μmol/L(r2=0.994 8) and a detection limit (S/N=3) of 0.049 μmol/L.The reproducibility of this method was evaluated by nine parallel trials with nine different electrodes,with a relative standard deviation (RSD) of 3.6%,indicating that a good reproducibility was obtained.The anti-interference performance of the sensor was also studied.Results showed that 5 000-fold K+,Na+,Cl-,citric acid and glucose,2 500-fold SO2-4,2 000-fold sucrose,8-fold tert-butylhydroquinone and 2-fold butylated hydroxytoluene produced no interference on the determination of BHA.To investigate the practical application value,the sensor was used to detect BHA in three kinds of biscuit samples.It was noteworthy that the results of samples obtained by this method were highly consistent with those obtained by high performance liquid chromatography,indicating a good accuracy.Furthermore,the recovery experiments for real samples at three concentration levels were carried out,and the recoveries were within the range of 95.6%-104%.The sensor was successfully applied to detect BHA in biscuit samples.Overall,the electrochemical sensor based on Au NPs@NU-901 composites,with good selectivity,sensitivity and accuracy for electrochemical oxidation of BHA,was successfully used in the quantitative determination of BHA in biscuit samples.This study provided a good demonstration for the application of noble metal nanoparticles and MOF composites in electrochemical field. |
| Key Words:metal organic frameworks Au nanoparticles(Au NPs) electrochemical sensor butylated hydroxyanisole biscuit |
| 引用本文：尹林华,史朝霞,胡玉斐，李攻科.基于Au NPs@NU-901电化学传感器检测饼干中丁基羟基茴香醚的研究[J].分析测试学报,2021,40(6):973-980. |
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