基于氧化石墨烯-Nafion修饰的玻碳电极检测血中辛弗林
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摘要
目的利用氧化石墨烯-Nafion修饰的玻碳电极对血浆样品中辛弗林进行测定。方法将分散在水中的氧化石墨烯(Graphene oxide,GO)和稀释成0.5%的Nafion溶液混合均匀后滴涂到玻碳电极上,并对缓冲溶液的种类等实验条件进行了优化,微分脉冲伏安法(Differential pulse voltammetry,DPV)测定辛弗林,结果在0.1mol·L~(-1) PB缓冲溶液,调节pH=7,电极修饰量为3μL时,辛弗林溶液氧化峰电流与其浓度在3.0×10~(-7)～1.0×10~(-5)mol·L~(-1)范围内呈良好的线性关系(r=0.9967),得检出限8.8×10~(-8)mol·L~(-1)。将该方法应用于血样中辛弗林的测定,其回收率在97.8%～102.6%之间。结论氧化石墨烯-Nafion修饰玻碳电极与未修饰玻碳电极相比,显著提高了辛弗林的氧化峰电流,提高了测定的灵敏度,所建立的方法可应用于人血样中辛弗林的痕量分析。
OBJECTIVE To determine synephrine in plasma sample by electrochemical method using Glassy Carbon Electrode modified with GO-Nafion.METHODS The GO was dispersed in water and mixed with 0.5% Nafion solution,and then dropped onto the surface of GCE.The eletrochemical behavior of synephrine at modified electrode was investigated by Differential Pulse Voltammetry(DPV).The exeperimental conditions including the buffer solution was optimized.RESULTS The pH value of 0.1 mol·L~(-1) PB buffer solution was adjusted to 7.0.3μL of GO-Nafionsuspension dropped onto the surface of GCE.Synephrine was determined using differential pulse voltammetry.The linear range of synephrine was 3.0×10~(-7)～1.0×10~(-5)mol·L~(-1) with the correlation coeffcient of 0.9967 and detection limit was 8.8×10~(-8)mol·L~(-1).This method was applied for the determination of synephrine in blood with the recoveries of 97.8%～102.6%.CONCLUSION The electrode modified with Go-Nafion improved significantly oxidation peak current of the synephrine with higher sensitivity than that of the bare GCE.This fabricated electrode was successfully applied for the trace analysis of synephrine in plasma sample.
OBJECTIVE To determine synephrine in plasma sample by electrochemical method using Glassy Carbon Electrode modified with GO-Nafion.METHODS The GO was dispersed in water and mixed with 0.5% Nafion solution,and then dropped onto the surface of GCE.The eletrochemical behavior of synephrine at modified electrode was investigated by Differential Pulse Voltammetry(DPV).The exeperimental conditions including the buffer solution was optimized.RESULTS The pH value of 0.1 mol·L~(-1) PB buffer solution was adjusted to 7.0.3μL of GO-Nafionsuspension dropped onto the surface of GCE.Synephrine was determined using differential pulse voltammetry.The linear range of synephrine was 3.0×10~(-7)～1.0×10~(-5)mol·L~(-1) with the correlation coeffcient of 0.9967 and detection limit was 8.8×10~(-8)mol·L~(-1).This method was applied for the determination of synephrine in blood with the recoveries of 97.8%～102.6%.CONCLUSION The electrode modified with Go-Nafion improved significantly oxidation peak current of the synephrine with higher sensitivity than that of the bare GCE.This fabricated electrode was successfully applied for the trace analysis of synephrine in plasma sample.
引文
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[14]张红梅,白妮,鲁杨.高效液相色谱法同时测定土地海苓煎颗粒中芒果苷、辛弗林的含量[J].中南药学,2014,12(03):265-267.
[15]冯怡,蔡贞贞,方兴德.薄层色谱扫描法测定青皮、枳实、枳壳中辛福林的含量[J].中成药研究,1985,8(03):28-29.
[16]Chen G,Zhang L,Zhao J,Ye J.Determination of hesperidin and synephrine in Pericarpium Citri Reticulatae by capillary electrophoresiswith electrochemicaldetection[J].Analytical And Bioanalytical Chemistry,2002,373(05):169-173.
[17]陆晓峰,王如健,彭国平,等.填充柱超临界流体色谱法测定枳实中辛弗林的含量[J].辽宁中医杂志,2006,33(02):222-223.
[18]郭长春.氧化石墨烯(GO)与磺化氧化石墨烯(SGO)的制备及其修饰电极电化学研究[D].青岛大学,2012.
[19]Lerf A,He H Y,Forster M.Structure of graphite oxide revisited[J].The Journal of Physical Chemistry B,1998,13(102):4477-4482.
[20]时克林,王晓蕾.Nafion膜修饰电极的制备及其通透性研究[J].化学分析计量,2011,12(01):41-44.
[2]方芳,董敏,朱红,等.枳实提取液对豚鼠心室肌细胞L型钙电流的影响[J].湖南医科大学学报,2003,28(04):353-356.
[3]王天山,潘扬,殷飞,等.马钱素与辛弗林对家兔重症失血性休克模型的作用[J].南京中医药大学学报(自然科学版),1999,15(06):345-346.
[4]官福兰,王如俊,王建华.枳壳及辛弗林对兔离体小肠运动的影响[J].中国药理与临床,2002,18(02):9-11.
[5]官福兰,王如俊,王建华.枳壳及辛弗林对小鼠胃排空、小肠推进功能的影响[J].现代中西医结合杂志,2002,11(11):1001-1003.
[6]钱亚琴.辛弗林的含量测定方法研究进展[J].中国药物警戒,2011,08(09):546-549.
[7]肖培根.新编中药志(第二卷)[M].北京:化学工业出版社,2002,459-460
[8]Satohs S J,Harry G.Preuss.Stereochemical and pharmacological differences between naturally occurring p-synephrine and synthetic p-synephrine[J].Journal of Functional Foods,2012,24(04):2-5.
[9]张明光.辛弗林及其类似物的合成研究[D].南京:南京林业大学,2008.
[10]彭彩云,徐运安,盛文斌,等.辛弗林分离检测方法研究进展[J].中医药导报,2009,15(03):99-108.
[11]LG Rossato,VM Costa,RP Limberger,et al.Synephrine:From trace concentration to massive consumption in weightloss[J].Food and Chemical Toxicology,2011,49(05):8-16.
[12]Government of Canada,Health Canada.Guidelines for the Use of Synephrine in Natural Health Products[J].Health Canada,2010,07(02):17-18.
[13]Stohs S J.Synephrine:From trace concentration to massive consumption in weight-loss[J].Food and Chemical Toxicology,2011,12(49):1472-1473.
[14]张红梅,白妮,鲁杨.高效液相色谱法同时测定土地海苓煎颗粒中芒果苷、辛弗林的含量[J].中南药学,2014,12(03):265-267.
[15]冯怡,蔡贞贞,方兴德.薄层色谱扫描法测定青皮、枳实、枳壳中辛福林的含量[J].中成药研究,1985,8(03):28-29.
[16]Chen G,Zhang L,Zhao J,Ye J.Determination of hesperidin and synephrine in Pericarpium Citri Reticulatae by capillary electrophoresiswith electrochemicaldetection[J].Analytical And Bioanalytical Chemistry,2002,373(05):169-173.
[17]陆晓峰,王如健,彭国平,等.填充柱超临界流体色谱法测定枳实中辛弗林的含量[J].辽宁中医杂志,2006,33(02):222-223.
[18]郭长春.氧化石墨烯(GO)与磺化氧化石墨烯(SGO)的制备及其修饰电极电化学研究[D].青岛大学,2012.
[19]Lerf A,He H Y,Forster M.Structure of graphite oxide revisited[J].The Journal of Physical Chemistry B,1998,13(102):4477-4482.
[20]时克林,王晓蕾.Nafion膜修饰电极的制备及其通透性研究[J].化学分析计量,2011,12(01):41-44.