摘 要

论文开展了ε-聚赖氨酸（ε-PL）银微电极方波伏安法（SWV）试验。结果表明：ε-PL循环伏安氧化还原峰不可逆；单因素法优化试验了ε-PL SWV的主要影响参数，支持电解质的较佳条件为pH＝6、0.2mol/L Na₂SO₄溶液；所得标准曲线的线性浓度范围为0~250mg·L^-1，线性方程为I_{(µA )}=0.082C_(mg·L-1) 0.2402，相关系数为0.9995，检出限为2.146 mg·L^-1。试验测定的100倍干扰物中，Na₂SO₄、NaCl、NH₄Cl对测定无明显干扰，KCl对测定有一定的干扰，葡萄糖、甘氨酸与抗坏血酸对测定有明显干扰。两周前后测得的ε-PL的氧化峰峰电流RSD%均小于2%，试验稳定性与重现性较好。橙汁、桃汁与混合果蔬三种试样的RSD%检测基本在5%以内，混合果蔬的加标回收率检测结果较好，但橙汁与桃汁检测结果相对不太理想。

关键词：ε-聚赖氨酸 银微电极 方波伏安法 测定

Silver microelectrodes coupled with square-wave voltammetry for the analysis of ε-polylysine

Abstract

In this paper, the ε-polylysine(ε-PL) silver electrode square-wave voltammetry(SWV) test was carried out. The results showed that the cycle voltammetric redox peak of ε-PL was irreversible; The single factor method optimized the main SWV influence parameters of ε-PL, and the better conditions for supporting electrolytes were pH = 6, 0.2 mol·L^-1 Na₂SO₄ solution; The linear concentration of the obtained standard curve ranged from 0 to 250 mg·L^-1, the linear equation was I_(μA) = 0.082 C_(mg·L-1) 0.2402, the correlation coefficient was 0.9995, and the detection limit was 2.146 mg·L^-1.Of the 100 times interference measured in the test,Na₂SO₄,

NaCl and NH₄Cl had no significant interference, KCl had certain interference, and glucose,

Glycine,and ascorbic acid had significant interference in the determination. The peak current RSD% of oxidation of ε-PL measured two weeks ago and two weeks later was less than 2%.And the stability and reproducibility of the test were better. RSD % test of orange juice, peach juice and mixed fruit and vegetables was basically within 5 %. The recovery rate of mixed fruits and vegetables was better, but the results of orange juice and peach juice were less satisfactory.

Key Words: ε-polylysine; silver microelectrodes; square-wave voltammetry; determination

目 录

摘要 I

ABSTRACT II

第一章 绪论 1

1.1 国内外研究进展 1

1.2 微电极分析概况 3

1.3 论文目的与意义 4

第二章 实验部分 5

2.1 试剂 5

2.2 仪器 5

2.3 实验方法 5

2.3.1 试剂配制及样品制备 5

2.3.2 电极的制备与使用 6

2.3.3 电化学试验 7

2.3.4 标准曲线的绘制 8

2.3.5 试样检测 8

2.3.6 干扰试验 9

2.3.7 稳定性与重现性 9

第三章 结果与讨论 10

3.1 循环伏安试验 10

3.2 方波伏安试验 10

3.2.1 方波起始电位 11

3.2.2 方波电位增量 12

3.2.3 方波振幅 13

3.2.4 方波频率 14

3.2.5 方波静置时间 15

3.3 支持电解质条件 15

3.3.1 支持电解质组分 15

3.3.2 溶液pH值 16

3.3.3 支持电解质浓度 16

3.4 标准曲线 17

3.5 试样检测 18

3.6 干扰试验 19

3.7 稳定性与重现性 20

第四章 结论与展望 21

参考文献 22

致谢 25

第一章 绪论

ε-聚赖氨酸（ε-Polylysine，ε-PL）是通过α-羧基和ε-氨基组成的酰胺键连接25-30个L-赖氨酸残基而成的聚合物^[1]。ε-PL的分子量约为3500-4500，无固定熔点，软化温度高于250℃，吸湿性强，稍有苦味，可溶于水、盐酸，微溶于乙醇，可生物降解，安全无毒，在1680-1640cm和1580-1520cm都有强烈的红外线吸收峰^[2]。

图1-1 ε-PL的化学结构

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