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机构地区:[1]河南工业大学化学化工学院,河南郑州450001
出 处:《分析测试学报》2011年第1期76-80,共5页Journal of Instrumental Analysis
基 金:河南省高校青年骨干教师基金资助项目(001135);河南省教育厅自然科学研究基金资助项目(2008B150006)
摘 要:用疏水性离子液体1-丁基-3-甲基眯唑六氟磷酸盐([BMIM]PF6)和纳米MnO2作修饰剂,通过壳聚糖(CHIT)的成膜效应,构置了玻碳修饰电极(【BMIM]PF6-MnO2-CHIT/GCE)。在Brinon—Robinson(B—R)缓冲液中研究了黄芩苷在修饰电极上的电化学行为,建立了测定黄芩胶囊中黄芩苷含量的新方法。黄芩苷在[BMIM]PF6-MnO2-CHIT/GCE上的循环伏安图出现一对灵敏、可逆的氧化还原峰,其峰电流响应是其在MnO2-CHIT/GCE上的2.6倍,峰电位差为0.062V,电子转移速率常数ks=0.258S。黄芩苷在[BMIM]PF6-MnO2-CHIT/GCE上的微分脉冲伏安扫描峰电流与其浓度的负对数在1.0×10^-91.0×10^-4mol/L范围内呈良好线性,检出限(S/N=3)为1.0×10^10mol/L。连续5次测定1.0×10^-8mol/L黄芩苷溶液的RSD为2.1%。该法用于黄芩苷药物的含量测定,加标回收率为95%~103%,结果满意。A new [ BMIM ] PF6 -MnO2 -CHIT/GCE modified electrode was fabricated via the chitosan(CHIT) fihning using hydrophobic ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate ( [ BMIM ] PF6 ) and nano-MnO2 as modifiers. In Britton - Robinson ( B - R) buffer, the electrochemical behavior of baicalin at [ BMIM ] PF6 - MnO2 - CHIT/GCE was studied, and a new method for the determination of baicalin in radix scutellariae was developed. The cyclic voltammetry curves of haicalin at [ BMIM ] PF6- MnO2- CHIT/GCE presented a pair of sensitive and reversible redox peaks. The peak current responsed at the proposed electrode was enhanced 2.6 folds higher than that at the MnO2 - CHIT/GCE, and the peak potential difference was 0. 062 V, the electron transfer rate constant ks was 0. 258 s^-1. The change of the oxidation peak current with baiealin concentration at [ BMIM]PF6 -MnO2 -CHIT/GCE was examined by differential pulse voltammetry. The calibration curve was linear in the concentration range of 1.0 × 10-9 - 1. 0× 10 5 mol/L with a detection limit (S/N=3) of 1.0× 10^10 mol/L. The relative standard deviation(n =5) of 1.0b 10-8 mol/L baicalin was 2. 1%. The method was applied in the determination of baicalin in samples with satisfactory results, and the spiked recoveries were in the range of 95% - 103%.
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