Determination of Benzoic Acid in Carbonated Beverage with Modified Glassy Carbon Electrode of Bis-Schiff Base Copper Complex
摘 要
利用溶液法制备双席夫碱铜配合物(M),采用电沉积法将制备的M沉积在玻碳电极(GCE)上制备了双席夫碱铜配合物修饰电极(M/GCE),用于测定碳酸饮料中的苯甲酸的含量。元素分析和红外光谱结果显示,试验成功制备了M;电沉积过程循环伏安曲线变化结果显示M已成功沉积在了GCE表面;扫描电镜(SEM)结果显示M/GCE表面已形成了一层聚合物膜。三电极体系选用M/GCE (工作电极)、饱和甘汞电极(参比电极)、铂丝电极(辅助电极);支持电解质采用0.1 mol·L-1 KCl溶液;电化学方法选用循环伏安法(CV),扫描速率为50 mV·s-1。结果表明,苯甲酸在M/GCE上的氧化峰电位和还原峰电位分别位于-0.007,-0.359 V附近,电极反应可逆性良好,受扩散控制。苯甲酸浓度与其对应的氧化峰电流在0.001 0~2.000 0 mmol·L-1内呈线性关系,检出限(3S/N)为0.27 μmol·L-1。将电极在4℃下放置7 d后,苯甲酸氧化峰电流下降了4.8%。以雪碧样品为基质进行了加标回收试验,回收率为97.6%~102%,测定值的相对标准偏差(n=5)为1.2%。
Abstract
Bis-Schiff base copper complex (M) was prepared by solution synthesis method, then M was deposited on the surface of glassy carbon electrode (GCE) by electrodeposition to prepared modified electrode of M (M/GCE). M/GCE was developed for determination of the content of benzoic acid in carbonated beverage. Elemental analysis and infrared spectroscopy showed that M was successfully prepared in the experiment; the curves of cyclic voltammetry (CV) of the electrodeposition process showed that M had been deposited on the GCE surface; scanning electron microscope (SEM) results showed that a polymer film had been formed on the surface of M/GCE. In the CV analysis for determination of the content of the benzoic acid, the three-electrode system was selected with M/GCE as working electrode, saturated calomel electrode as reference electrode, platinum wire electrode as auxiliary electrode and 0.1 mol·L-1 KCl solution as the supporting electrolyte at the scan rate of 50 mV·s-1. It was shown by results that the oxidation peak potential and reduction peak potential of benzoic acid on M/GCE were ca. -0.007, -0.359 V, respectively. The electrode reaction was reversible and controlled by diffusion. Linear relationship between concentrations and their respective oxidation peak current of benzoic acid found was in the range of 0.001 0-2.000 0 mmol·L-1, with detection limit (3S/N) of 0.27 μmol·L-1. After placing the electrode at 4℃ for 7 d, the oxidation peak current of benzoic acid decreased by 4.8%. A sprite sample was used as a matrix to made a spiked recovery test, giving recoveries of 97.6%-102%; and RSD (n=5) of the measured value found was 1.2%.
中图分类号 O657.15 DOI 10.11973/lhjy-hx202008001
所属栏目 试验与研究
基金项目 广西特聘专家专项经费资助(2401007012)
收稿日期 2019/11/8
修改稿日期
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作者单位点击查看
联系人作者刘峥(lisa4.6@163.com)
备注梁楚欣,硕士研究生,研究方向为有机合成与配位物合成
引用该论文: LIANG Chuxin,LIU Zheng,CHEN Zesheng,FENG Weiyi,LI Haiying,ZHANG Shufen. Determination of Benzoic Acid in Carbonated Beverage with Modified Glassy Carbon Electrode of Bis-Schiff Base Copper Complex[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(8): 845~850
梁楚欣,刘峥,陈则胜,冯炜怡,李海莹,张淑芬. 双席夫碱铜配合物修饰玻碳电极用于碳酸饮料中苯甲酸的测定[J]. 理化检验-化学分册, 2020, 56(8): 845~850
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参考文献
【1】LI H, LONG R Q, TONG C Y, et al. Shell thickness controlled hydrophilic magnetic molecularly imprinted resins for high-efficient extraction of benzoic acids in aqueous samples[J]. Talanta, 2019,194:969-976.
【2】TIMOFEEVA I, KANASHINA D, KIRSANOV D, et al. A heating-assisted liquid-liquid microextraction approach using menthol:Separation of benzoic acid in juice samples followed by HPLC-UV determination[J]. Journal of Molecular Liquids, 2018,261:265-270.
【3】SUN X D, ZHU K, LIU J B, et al. Terahertz spectroscopy determination of benzoic acid additive in wheat flour by machine learning[J]. Journal of Infrared, Millimeter, and Terahertz Waves, 2019,40(4):466-475.
【4】帅放文,王向峰,雷玉萍,等.四种苯甲酸检测方法比较研究[J].中国食品添加剂, 2016(4):161-165.
【5】HEO Y J, LEE K J. Application of micellar electrokinetic capillary chromatography for the determination of benzoic acid and its esters in liquid formula medicines as preservatives[J]. Journal of Pharmaceutical and Biomedical Analysis, 1998,17(8):1371-1379.
【6】KOKYA T A, FARHADI K, KALHORI A A. Optimized dispersive liquid-liquid microextraction and determination of sorbic acid and benzoic acid in beverage samples by gas chromatography[J]. Food Analytical Methods, 2012,5(3):351-358.
【7】JAWAID S, TALPUR F N, NIZAMANI S M, et al. Rapid in situ esterification method for the determination of benzoic acid in dairy milk by GC-FID[J]. Food Analytical Methods, 2015,8(6):1477-1483.
【8】GUARINO C, FUSELLI F, MANTIA A L, et al. Development of an RP-HPLC method for the simultaneous determination of benzoic acid, sorbic acid, natamycin and lysozyme in hard and pasta filata cheeses[J]. Food Chemistry, 2011,127(3):1294-1299.
【9】DING M Z, PENG J, MA S L, et al. An environment-friendly procedure for the high performance liquid chromatography determination of benzoic acid and sorbic acid in soy sauce[J]. Food Chemistry, 2015,183:26-29.
【10】KAVRAKOVSKI Z S, RAFAJLOVSKA V G. Development and validation of thin layer chromatography method for simultaneous determination of seven chlorophenoxy and benzoic acid herbicides in water[J]. Journal of Analytical Chemistry, 2015,70(8):995-1000.
【11】WANG J P, GUO X F, JIA L H. A simple method for the determination of benzoic acid based on room temperature phosphorescence of 1-bromopyrene/γ-cyclodextrin complex in water[J]. Talanta, 2017,162:423-427.
【12】吴勤民.荧光光谱法和紫外分光光度法在发酵调味品中苯甲酸含量测定中的应用和比较[J].中国调味品, 2010,35(1):78-80.
【13】郭征楠,刘峥,魏席,等.噻吩-2-甲醛缩L-半胱氨酸Schiff碱共价结合CdTe量子点修饰金电极循环伏安法测定柠檬黄[J].食品科技, 2016,41(1):299-306.
【14】梁楚欣,刘峥,梁秋群,等.含羧基双席夫碱及其铜(Ⅱ)配合物的合成、晶体结构及其性质[J].无机化学学报, 2019,35(7):1130-1138.
【15】AMER A A, ILIKTI H, BEYENS C, et al. Elaboration of new modified electrodes (MEs) by electropolymerization of Cu(Ⅱ)-Schiff base complexes bearing pyrrole moieties:Application in electroreduction of acetophenone and carbon dioxide[J]. European Polymer Journal, 2019,112:569-580.
【16】南明君,顾婷婷,周洋,等.DNA-Fe配合物生物聚合离子膜修饰GCE的制备及其用作过氧化氢电化学传感器的研究[J].理化检验-化学分册, 2017,53(7):753-758.
【17】MARTIN C S, MACHINI W B S, TEIXEIRA M F S. Electropolymerization using binuclear nickel(Ⅱ) Schiff base complexes bearing N4O4 donors as supramolecular building blocks[J]. RSC Advances, 2015,5(50):39908-39915.
【18】CAI Z Y, PEI L Z, XIE Y K, et al. Electrochemical determination of benzoic acid using CuGeO3 nanowire modified glassy carbon electrode[J]. Measurement Science and Technology, 2013,24(9):095701-095701.
【2】TIMOFEEVA I, KANASHINA D, KIRSANOV D, et al. A heating-assisted liquid-liquid microextraction approach using menthol:Separation of benzoic acid in juice samples followed by HPLC-UV determination[J]. Journal of Molecular Liquids, 2018,261:265-270.
【3】SUN X D, ZHU K, LIU J B, et al. Terahertz spectroscopy determination of benzoic acid additive in wheat flour by machine learning[J]. Journal of Infrared, Millimeter, and Terahertz Waves, 2019,40(4):466-475.
【4】帅放文,王向峰,雷玉萍,等.四种苯甲酸检测方法比较研究[J].中国食品添加剂, 2016(4):161-165.
【5】HEO Y J, LEE K J. Application of micellar electrokinetic capillary chromatography for the determination of benzoic acid and its esters in liquid formula medicines as preservatives[J]. Journal of Pharmaceutical and Biomedical Analysis, 1998,17(8):1371-1379.
【6】KOKYA T A, FARHADI K, KALHORI A A. Optimized dispersive liquid-liquid microextraction and determination of sorbic acid and benzoic acid in beverage samples by gas chromatography[J]. Food Analytical Methods, 2012,5(3):351-358.
【7】JAWAID S, TALPUR F N, NIZAMANI S M, et al. Rapid in situ esterification method for the determination of benzoic acid in dairy milk by GC-FID[J]. Food Analytical Methods, 2015,8(6):1477-1483.
【8】GUARINO C, FUSELLI F, MANTIA A L, et al. Development of an RP-HPLC method for the simultaneous determination of benzoic acid, sorbic acid, natamycin and lysozyme in hard and pasta filata cheeses[J]. Food Chemistry, 2011,127(3):1294-1299.
【9】DING M Z, PENG J, MA S L, et al. An environment-friendly procedure for the high performance liquid chromatography determination of benzoic acid and sorbic acid in soy sauce[J]. Food Chemistry, 2015,183:26-29.
【10】KAVRAKOVSKI Z S, RAFAJLOVSKA V G. Development and validation of thin layer chromatography method for simultaneous determination of seven chlorophenoxy and benzoic acid herbicides in water[J]. Journal of Analytical Chemistry, 2015,70(8):995-1000.
【11】WANG J P, GUO X F, JIA L H. A simple method for the determination of benzoic acid based on room temperature phosphorescence of 1-bromopyrene/γ-cyclodextrin complex in water[J]. Talanta, 2017,162:423-427.
【12】吴勤民.荧光光谱法和紫外分光光度法在发酵调味品中苯甲酸含量测定中的应用和比较[J].中国调味品, 2010,35(1):78-80.
【13】郭征楠,刘峥,魏席,等.噻吩-2-甲醛缩L-半胱氨酸Schiff碱共价结合CdTe量子点修饰金电极循环伏安法测定柠檬黄[J].食品科技, 2016,41(1):299-306.
【14】梁楚欣,刘峥,梁秋群,等.含羧基双席夫碱及其铜(Ⅱ)配合物的合成、晶体结构及其性质[J].无机化学学报, 2019,35(7):1130-1138.
【15】AMER A A, ILIKTI H, BEYENS C, et al. Elaboration of new modified electrodes (MEs) by electropolymerization of Cu(Ⅱ)-Schiff base complexes bearing pyrrole moieties:Application in electroreduction of acetophenone and carbon dioxide[J]. European Polymer Journal, 2019,112:569-580.
【16】南明君,顾婷婷,周洋,等.DNA-Fe配合物生物聚合离子膜修饰GCE的制备及其用作过氧化氢电化学传感器的研究[J].理化检验-化学分册, 2017,53(7):753-758.
【17】MARTIN C S, MACHINI W B S, TEIXEIRA M F S. Electropolymerization using binuclear nickel(Ⅱ) Schiff base complexes bearing N4O4 donors as supramolecular building blocks[J]. RSC Advances, 2015,5(50):39908-39915.
【18】CAI Z Y, PEI L Z, XIE Y K, et al. Electrochemical determination of benzoic acid using CuGeO3 nanowire modified glassy carbon electrode[J]. Measurement Science and Technology, 2013,24(9):095701-095701.
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