团聚状纳米AuPd修饰的H2O2生物传感器研究

采用微胶束法室温条件下制备团聚状的AuPd合金纳米粒子,使用紫外可见光谱(UV-vis),透射电镜(TEM),X-射线粉末衍射(XRD)和X-射线能量色散谱(EDS)表征团聚结构AuPd合金纳米粒子的形貌、尺寸、结构和组成。用制备的AuPd纳米粒子修饰辣根过氧化物酶玻碳电极,制备无电子媒介的过氧化氢生物传感器HRP/AuPd/GCE。使用循环伏安法和计时电流法表征了HRP/AuPd/GCE对H2O2的检测性能。实验结果表明:该传感器对H2O2具有良好的检测性能和稳定性,在H2O2浓度为1×10-7mol/L～5×10-3mol/L范围内检测电流与H2O2浓度有线性关系,线性相关系数R2=0.995 01,检出限为7.6×10-7mol/L。     

AuRu纳米粒子修饰的辣根过氧化物酶传感器研究

采用反向胶束法在室温下合成出AuRu纳米粒子,使用X射线衍射(XRD)、能量色散X射线光谱 (EDS)、高分辨透射电镜(HRTEM)表征其结构、组成和形貌,制备其修饰辣根过氧化物酶传感器(HRP/AuRu/GC)。使用循环伏安法(CV)和计时电流法(i-t)研究该传感器对H2O2的检测性能。结果表明：HRP/AuRu/GC对H2O2检测具有高的灵敏度和稳定性,在H2O2浓度为1×10-7～1×10-3mol/L范围内检测电流与浓度的负对数成线性关系,线性相关系数R2＝0.9959,检出限为5.02×10-8mol/L。电极使用1个月后其响应电流为原来的91.54%。     

SiO2球腔微电极阵列过氧化氢传感器制备及应用

将微过氧化物酶-11(MP-11)直接固定于二氧化硅球腔微电极阵列,制备一种新型电化学过氧化氢(H2O2)生物传感器。采用Langmuir-Blodgett技术在氧化铟锡(ITO)电极表面制备聚苯乙烯(PS)微球阵列,并以此阵列为模板采用溶胶-凝胶法在ITO电极上制备二氧化硅(SiO2)球腔阵列,最后将微过氧化物酶-11作为氧化还原模型蛋白直接吸附于球腔内,制得MP-11/SiO2球腔阵列/ITO电极。该电极对H2O2响应快速灵敏,可作为电流型H2O2电化学生物传感器,其线性范围为7.06×10-6～4.02×10-2mol/L,检出限为3.0×10-7mol/L,米氏常数为0.916mmol/L。将该法用于食品样品中的H2O2的检测,回收率在94%～97%之间,效果良好,可为食品中残存的H2O2检测提供一种方法。     

聚中性红辣根过氧化物酶传感器测定啤酒中的过氧化氢

制备了以电子媒介体聚中性红固定辣根过氧化物酶(HRP)的生物传感器,采用循环伏安法对该传感器的性能进行了研究。结果表明,辣根过氧化物酶在该电极上实现了稳定的直接电子转移反应,传感器在H2O2浓度为3.18×10-8～3.18×10-3mol/L的范围内具有良好的线性相关性,检出限为6.36×10-9mol/L。应用于啤酒中H2O2的测定,回收率为88.5%～98.6%。     

酱油中氨基酸的快速极谱测定

用线性扫描极谱法研究了在B-R缓冲溶液中茚三酮的极谱行为.实验表明,以pH=4.58的B-R缓冲溶液和0.1 mol/L的KCl溶液作为底液,茚三酮产生还原波,其二阶导数峰电位为-0.874V(vs.SCE),峰电流与其浓度在1.12×10-6～3.36×10-4 mol/L浓度范围内呈线性关系,线性方程为i"p(nA/s2)=114.5 7.393×106 c mol/L,相关系数为0.9927.研究了茚三酮与氨基酸相互作用后的极谱行为.结果表明,加入氨基酸后峰电位没有变化,峰电流随氨基酸的浓度增大而减小.对L-组氨酸在6.10×10-5～6.10×10-4 mol/L和1.22×10-6～1.22×10-5 mol/L的浓度范围内线性方程分别为i"p(nA/s2)= 147.6～2.150×104c mol/L,相关系数为0.9977;和i"p(nA/s2)=174.8～1.604×106 c mol/L,相关系数为0.9961.用标准加入法测定了市售酱油中氨基酸的含量.     

复合纳米微粒修饰丝网印刷电极的一次性过氧化氢生物传感器研究

构建纳米金(Au)-石墨烯(GS)-辣根过氧化物酶(HRP)-Nafion纳米复合物修饰丝网印刷电极(SPCEs)的一次性过氧化氢生物传感器,并用于过氧化氢的测定。采用化学镀金方法于SPCEs表面形成Au,然后将GS、HRP和Nafion组成的复合物涂覆于SPCEs/Au表面,构建SPCEs/Au/GS/HRP/Nafion电极,采用扫描电镜(SEM)表征化学镀金、GS和电极的制备过程,采用循环伏安(CV)法和计时电流(i-t)法研究H2O2的电化学性质。在优化的实验条件下,该电极能实现HRP的直接电子传递,对H2O2有显著的电催化作用,在2.0×10-5～2.5×10-3mol/L浓度范围内对H2O2有良好的线性响应,线性相关系数为0.9994,检测限为1.2×10-5mol/L。该传感器灵敏快速、制备容易、样品用量少、可抛弃、抗干扰性强,有望用于食品中痕量HO残留的检测。     

多壁碳纳米管/磷钨酸复合膜修饰电极差分脉冲伏安法测定苏丹红Ⅳ

制备了多壁碳纳米管/磷钨酸复合膜修饰电极,研究了该修饰电极对苏丹红Ⅳ的电催化作用,考察了富集电位、富集时间、脉冲宽度、脉冲振幅和支持电解质等因素对苏丹红Ⅳ响应的影响。在优化实验条件下,苏丹红Ⅳ浓度为1×10-6mol/L～4×10-5mol/L范围内,差分脉冲伏安峰电流与苏丹红Ⅳ的浓度呈现良好的线性关系,相关系数R=0.995,检出限为8×10-7mol/L。共存的多种离子、β-胡萝卜素等不干扰测定。     

基于金钯纳米合金修饰的过氧化氢传感器的研制

研制金钯合金纳米粒子修饰的特异性定量检测食品中过氧化氢残留量的过氧化氢传感器。以比表面积大、生物相容性好、具有优良电催化性能的金钯合金纳米粒子固定辣根过氧化物酶于玻碳电极,制得过氧化氢传感器电极。通过循环伏安法及交流阻抗法表征电极在组装过程中的电化学特性,利用计时电流法对传感器性能进行考察。研究表明：该传感器测定H2O2的线性范围为1×10-7～5×10-3mol/L,检测限为8.0×10-7 mol/L,对H2O2具有较好的催化还原活性和良好的检出性能。该传感器制作简单、成本低廉、可重复性强,可用于快速定量检测食品中过氧化氢残留量。     

用于有机磷农药检测的植物酯酶生物传感器的研究

报道了一种用于有机磷农药检测的电流型生物传感器.从小麦中提取植物酯酶,纯化后作为生物传感器的酶源,以CuTAPC/SWCNT/GC修饰电极为基体电极,采用气相沉积法制备TiO2凝胶,通过凝胶包埋法制备植物酯酶生物传感器.该传感器具有良好的稳定性和重现性.当对硫磷、辛硫磷和氧化乐果浓度分别在0.5×10-9～1×10-5、10-9～10-5、0.5 × 10-8～10-5 mol/L范围内时,抑制率与其浓度的对数呈线性关系,检测限分别为3.24×10-10、1.26×10-9、6.60×10-9mol/L.     

用辣根过氧化物酶生物传感器测定啤酒中的过氧化氢

用一种新型的壳聚糖(CS)/聚乙烯吡咯烷酮(PVP)复合膜固定辣根过氧化物酶(HRP),以乙二醛作交联剂,二茂铁(Fc)作媒介体,制备过氧化氢生物传感器。采用循环伏安法对该传感器的性能进行研究。结果表明,传感器在H2O2浓度为3.00×10-8～3.00×10-4 mol/L的范围内具有良好的线性相关性。使用SBA-50生物传感分析仪测定啤酒中的H2O2,回收率为97.6%～101.8%。     

辣根过氧化物酶传感器的研究──对苯二酚为电子传递体

用牛血清白蛋白和戊二醛把辣根过氧化物酶固定在对苯二酚修饰的电极上,制成过氧化氢传感器。该酶电极对过氧化氢有良好的响应,对苯二酚还原电流的增值与过氧化氢浓度在2×10（－7）～2×10（－3）mol／L范围内有良好的线性关系,该传感器灵敏度高,检出限为10（－7）mol／L,对过氧化氢的响应时间小于25s。     

Electrochemical Determination of Tert-Butyl Hydroquinone in Edible Oil Samples at Poly (Crystal Violet) Modified Glassy Carbon Electrode

The synthetic phenolic antioxidant tert-butyl hydroquinone (TBHQ) is frequently associated to adverse health effects. A polymerized film of crystal violet (CV) was prepared on the surface of a glass carbon electrode (GCE) by electropolymerization in alkaline solution, and then the modified electrode was successfully used to determine TBHQ. This electrode was characterized by scanning electron microscopy and electrochemical impedance spectra. The voltammetric behavior of TBHQ over an extended pH range using cyclic voltammetry at poly (crystal violet) modified glassy carbon electrode (PCV/GCE) was also studied. The resulting electrode exhibited excellent electrocatalytic activity towards the oxidation of TBHQ, and this was confirmed by the observed increased redox peak currents and shifted potentials. The electrochemical sensor can be applied to the quantification of TBHQ with a linear range covering 5?×?10^?7–1?×?10^?4 mol?·?L^?1 (with a correlation coefficient of 0.9969) and the limit detection was 3?×?10^?8 mol?·?L^?1(S/N?=?3). The recovery was between 97.1 and 102 % in edible oil samples. The electrochemical sensor method was also compared with a HPLC method, which proves its capability in commercial market surveillance.     

Electrochemical oxidation of hydroquinone, resorcinol, and catechol on boron-doped diamond anodes

The electrochemical oxidation of aqueous wastes polluted with hydroquinone, resorcinol, or catechol on boron-doped diamond electrodes has been studied. The complete mineralization of the organic waste has been obtained independently of the nature of each isomer. No aromatic intermediates were found during the treatment, and solely aliphatic intermediates (carboxylic acids C4 and C2, mainly) were detected in the three cases. Although as from the bulk electrolyses study no differences in the electrochemical oxidation of dihydroxybenzenes seem to exist, different voltammetric behavior between resorcinol and the other two isomers was obtained in the voltammetric study. Catechol and hydroquinone have a reversible quinonic form, and a cathodic reduction peak appears in their voltammograms. The characterization of the first steps in the electrochemical oxidation of the three dihydroxybenzenes showed the formation of a larger number of intermediates in the oxidation of catechol, although no carbon dioxide was detected in its oxidation. Conversely, the oxidation of resorcinol and hydroquinone lead to the formation of important concentrations of carbon dioxide. The nondetection of aromatic intermediates, even if small quantities of charge are passed, confirms that the oxidation must be carried out directly on the electrode surface or by hydroxyl radicals generated by decomposition of water.     

碳纳米管-壳聚糖复合物免疫传感器检测牛奶中的青霉素

建立了一种高灵敏度阻抗电化学免疫分析法测定青霉素的方法。利用层层自组装技术将多壁碳纳米管（MWCNTs）,壳聚糖（CS）,和Ⅷ冲标记青霉素抗体（HRP．Ab＊）共固定于玻碳电极表面,利用HRP可以催化H202的还原进一步促进对苯二酚的氧化,从而引起阻抗的变化,然后根据电流的变化从而实现了对牛奶中青霉素的定量测量。对于牛奶样品,需要盐析以除去其蛋白质和脂肪,同时对缓冲液的pH、免疫温度和时间都进行了优化。实验表明,在优化条件下,该传感器的响应电流与青霉素的浓度在0．05～5μgL-1范围内有较好的线性关系,相关系数为0．9853,检测限是1．05μgL皿。最后,通过和酶联免疫法（ELISA）对比,可知该法测定青霉素灵敏度高,重复性好,特异性高,可适合用于检测牛奶样品中的青霉素残留。     

MnO2/ZnO/GCE电化学传感器的构建及对蜂蜜中磺胺甲恶唑的检测

为快速检测蜂蜜中磺胺甲恶唑(sulfamethoxazole,SMZ)的残留,将水热法制备的氧化锌(ZnO)及共沉淀法制备的二氧化锰(MnO₂)材料复合于玻碳电极(GCE)上,构建了MnO₂/ZnO/GCE电化学传感器用于检测SMZ。采用扫描电镜(SEM)及红外光谱(FT-IR)对复合材料的形貌、结构进行表征。利用差分脉冲伏安法(DPV)对复合材料的比例、修饰量进行探究,从而对传感器的构建条件进行优化。并采用差分脉冲伏安法(DPV)及循环伏安法(CV)对缓冲溶液pH、扫描速率等检测条件进行考察。结果表明,当m(ZnO):m(MnO₂)质量比为1:0.6、MnO₂/ZnO复合材料修饰量为1.7×10-3 mg/mm2、缓冲溶液pH为8、扫描速率为30 mV/s时,该传感器对SMZ具有良好的检测效果。在0.3～100μmol/L范围内,峰电流与SMZ浓度呈良好的线性关系,其线性方程为Ip=0.0843 c+4.5168(R2=0.9916),检测限为0.39μmol/L,定量限为1.30μmol/L。将...     

Effects of Processing Conditions and Antioxidants on the Oxidative Stability and Carbon Dioxide Formation in Low Fat Dry Milk

The effects of different processing methods and antioxidants on the oxidative stability and carbon dioxide formation in low fat dry milk at 65°C for 8 days were determined by measuring volatile compound formation, oxygen disappearance, and carbon dioxide formation in the gas-tight sample bottle by gas chromatography. Foam spray dried or steam jacketed centrifugal wheel atomization dried milks had significantly less (P < 0.05) volatile compound formation, oxygen depletion, and carbon dioxide formation than conventional spray dried milks. Dry milks containing 100 ppm propyl gallate showed significantly less (P <0.05) oxygen disappearance, volatile compound formation, and carbon dioxide formation than dry milks containing 100 ppm butylated hydroxyanisole or tertiarybutyl hydroquinone during storage.     

基于Nafion/Hb/Fe3O4@Cs/GCE传感器检测油炸食品中丙烯酰胺

目的 制备Nafion/Hb/Fe3O4@Cs/GCE传感器, 并应用于油炸食品中丙烯酰胺(acrylamide, AM)的检测分析。方法 制备Fe3O4@碳球纳米复合材料(Fe3O4 carbon sphere nanocomposites, Fe3O4@Cs), 并复合Nafion和血红蛋白(hemoglobin, Hb), 以玻碳电极(glassy carbon electrode, GCE)为工作电极制备Nafion/Hb/Fe3O4@Cs/GCE传感器, 通过对固载方式、Hb固载量、加成温度以及加成时间的优化确定Nafion/Hb/Fe3O4@Cs/GCE对丙烯酰胺进行定量检测的最佳检测条件。结果 Fe3O4@Cs导电性良好, 能显著提高Nafion/Hb/Fe3O4@Cs/GCE传感器的灵敏度。AM与Hb的加成率与其浓度负对数在1×10?5~1×10?9 mol/L范围内呈良好的线性关系, 线性方程为Y=?5.254X+60.01 (X为AM浓度的负对数), r2=0.9973, 检出限为2.134×10?10 mol/L, 加标回收率在95.6%~98.4%之间, 相对标准偏差小于1.45%。结论 该方法简单、方便快捷, 适用于油炸食品中AM的定量分析。     

碳纳米管修饰电极差分脉冲伏安法测定微量Pb2+

以碳纳米管(CNT)修饰玻碳电极为工作电极,于-1.0V吸附富集后差分脉冲伏安法测定水中微量铅离子,实验优化了支持电解质、pH、CNT用量。从富集电位正向扫描至0V,在-0.58V处产生铅的阳极溶出峰,溶出峰电流值与Pb2+浓度在0.005～1μg/mL范围内呈良好的线性关系,线性方程为y=16.0911x-0.2284(r=0.9962),检测下限为0.005μg/mL,回收率为95.4%～105.5%,6次重复测定RSD为1.69%。碳纳米管显著改善了铅离子检测信号,所提出的检测方法简单、灵敏、快速、选择性好,能应用于实际样品测定。     

石墨烯/四氧化三钴电化学传感器的建立及饼干中香兰素检测分析

本文将石墨烯（GR）滴涂在玻碳电极（GCE）后,再通过循环伏安法电聚合氧化Co（COOH）₂制得Co₃O₄/GR/GCE修饰电极作为食品中检测香兰素的新型电化学传感器。通过扫描电镜技术对Co₃O₄/GR复合纳米材料进行了表征并优化了实验条件。结果表明,当1 mg/mL GR滴涂量为8 μL,Co（COOH）₂聚合圈数为20圈,0.1 mol/L pH 4.5磷酸缓冲溶液中,香兰素在该传感器下线性关系良好（0.1～80 μmol/L）,线性方程为:I_p （μmol/L）=0.1518C+0.5103 （R2=0.997）,检测限为0.033 μmol/L （S/N=3）。将此方法应用于饼干样品中香兰素检测,回收率良好,相对标准偏差仅1.47%。综上,该电化学传感器灵敏度较高、稳定性良好,在实际样品检测中具有可行性,拥有广阔的应用前景。     

Tannic acid assisted copper oxide nanoglobules for sensitive electrochemical detection of bisphenol A

This study describes the development of an electrochemical sensor system for the determination of bisphenol A using tannic acid functionalized CuO nanoglobules. The utilized tannic acid acted simultaneously as both bio-compatible template and functionalizing agent for the as-synthesised CuO nanostructures. The excellent synergy of high surface area and favorable interactions between the moieties of tannic acid and bisphenol A molecules enabled sensitive electrochemical oxidation of bisphenol A within wide detection window (0.1–5.5 µM) and limit of detection estimated to be 0.01 µM. Moreover, the sensor exhibited satisfactory stability and strong anti-interference capability when evaluated against common interferents molecules such as phenol, hydroquinone, and 4-nitrophenol.