【作者】 于浩；

【导师】 郑建斌；

【作者基本信息】 西北大学 ， 分析化学， 2002， 硕士

【摘要】 本论文主要开展几种药物的示波行为及其应用的研究。该研究对探索示波法响应药物的机理，扩大示波分析应用范围，丰富药物分析方法等有重要意义。全文共分四章，作者的主要贡献有以下几个方面： 一、研究了红霉素和吉非罗齐的示波计时电位行为，并分别建立了测定其含量的二次微分简易示波伏安法。发现在0.2mol／L NaOH底液中，红霉素在示波计时电位曲线（dE／dt-E曲线）阴极支-1.36V和-1.52V产生两个切口，且可以从示波器上观察到-1．52V的切口深度逐渐降低，而在-1.36V产生另一个切口的变化过程。通过与紫外分光光度法和循环伏安法研究的结果比较认为：在碱性溶液中红霉素在示波图上产生的两个切口分别是其分子和水解产物还原产生的。这一研究表明，示波计时电位法在用于某些化学反应过程监测方面有其独特的优越性。 二、在0.2mol／L KCl+0.2mol/L H₃BO₃底液中，黄连素于dE／dt-E曲线阴极支-1.49V、-1.78V处产生两个不可逆的切口，其中第一个切口可用于黄连素的定量分析。当黄连素浓度在1.3×10^-6～1.0×l0^-5mol／L范围内时与第一切口的二次微分简易示波伏安图上峰高有线性关系；检出限为8×10（-7）mol／L；对4.0×10（-6）mol／L黄连素进行5次测定的RSD为1.5％，样品的平均回收率为100.8％。通过对示波计时电位法与单扫描极谱法和循环伏安法研究结果的比较认为：-1.49V的切口是由于黄连素的电极反应产物吸附而产生的类似于单扫描极谱法中的吸附前波性质的切口，-1.78V的切口是由于黄连素电还原时产生的扩散型切口。 三、研究了葛根素、染料木素在NaOH溶液中的示波行为并建立了二次微分简易示波伏安法测定中药葛根及心可舒片剂中葛根素含量和大豆提取物中染料木素的新方法。测定葛根素的线性范围为2.5×10^-6～3.5×10^-5mol／L；检出限为1.2×10^-6mol/L；对9.0×10^-6mol／L葛根素进行5次测定的RSD为1.5％，测定中药葛根及心可舒片剂中的平均回收率分别为96.03％和93.43％。测定染料木素的线性范围为3.0×10^-6～4.4×10^-5mol／L，检出限为1.5×10^-6mol／L，样品的平均回yK4ktMMtW－－－ed收率为98刀％。本方法的特点为：仪器简单、方法简便快速、无需通氮除氧。 四、在 0．05 mo凡 NazB。O，一 0．05 mo凡 KNO。底液中，用示波计时电位法研究了Cd”与芦丁形成的配合物的示波行为，并与其单扫示波极谱、循环伏安行为进行了比较。实验结果表明：Cd”与芦丁形成的配合物在dEut－E曲线阴极支心厂SV产生的切口具有配合吸附波性质。这一示波特性可分别用于Cdh、芦丁及川”含量的测定。测定 CdZ＼芦丁和川“的线性范围分别为 2．4X10”‘～3．5X10－5mow、l刀xlo”‘～ 8刀x10－’mo几、l．sxlo”‘～ 1．Zxlo＊ moljL，检出限分别为1．2x10－6、6．oxlo－’mo凡和6．0x10－’mo皿。该法用于药槐角中的芦丁及胃舒平片中铝的含量测定，平均回收率分别为gi．17％和99．54％。更多还原

【Abstract】 The oscillographic behaviors and its application of several medications were studied in this thesis. This investigation is very useful for probing the oscillographic mechanism of medication, broadening the range of oscillographic analysis and developing analytical methods for medication. This thesis consisted of four chapters, and main contents are as follows:l.The oscillographic behaviors of erythromycin and gemfibrozil were studied, and second order differential simple oscillographic voltammetry for the determination of erythromycin and gemfibrozil was founded. Experimental results showed that there are two incisions of erythromycin at -1.52V and -1.36V on the cathodic branch of d?dt - E curve in different pH solution. Once erythromycin is added into 0.2 mol/L NaOH, an incision at -1.52V appeared immediately on the oscillogram, and the incision depth decreased gradually and disappeared eventually with increase of time, whereas a new incision at -1.36V appeared and reached a stable height. The whole process could be observed on the screen of cathode ray oscillograph. The mechanism of two incisions was investigated by comparing with ultraviolet spectrography and cyclic voltammetry, which is likely to be caused by the reduction of erythromycin and its hydrolysate in strong alkaline solution. The study showed that oscillographic chonopotentiometry could be applied to monitoring the process of some chemical reactions.2. Two irreversible incision of berberine were observed on the cathodic branch of dE/dt - E curve in 0.2mol/L HsBOs - 0.2 mol/L KCI solution, and the incision potential was -1.49V and -1.78V, respectively. Based on the oscillographic characteristic of the first incision, second order diffenrential simple oscillographic voltammetry for the determination of berberine in capsule was founded. The linear range and detection limit for berberine was 1.3X10"6 ~ 1.0X10"5 mol/L, and 1.0X10"6 mol/L, respectively. The relative standard deviation and the average recovery in thesample was 1.5%(n=5) and 100.8%, respectively. Moreover, the mechanism of two incisions was investigated by comparing. The experimental results investigated with oscillographic method, single sweep poloragraphy and cyclic voltammetry showed that the first incision (-1.4 9V) was related to the strong adsorption of reductive production, and another (- 1.49V) was related to the diffusion of reactant.3. Based on the oscillographic characteristic of genistein and puerarin, second order differential simple oscillographic voltammetry for the determination of genistein and puerarin in medication was founded. The linear range was 3.0* 10~6 ~ 4.4* 10~5 mol/L and 2.5X10"6 - 3.5X10"5 mol/L, respectively. The detection limit for genistein and puerarin was 1.5x10"* mol/L and 1.2 X10"6 mol/L, respectively. Compared with other methods, simple oscillographic voltammetry with second order differential was a convenient method due to its cheap equipment and rapid measurement.4. The oscillographic behavior of the cooperation formed between rutin and Cd2+ was investigated in 0.05 mol/L Na2B4O7 - 0.05 mol/L KNOa buffer solution, and the oscillographic behavior was compared with single sweep poloragraphy and cyclic voltammetry. The experimental results showed that the incision caused by the cooperation at -0.75V of the cathodic branch on dE/dt-E curve has adsorption property. The oscillographic characteristic for the cooperation can be applied to the determination of Cd2+, rutin and A13+, respectively. The linear range for the determination of Cd2+, rutin and A13+ was 2.4*10"6 ~ 3.5*10’5 mol/L, l.QxlO"6 ~ S.OxlO"5 mol/L and 1.8*10"6 mol/L ~ 1.2x10"" mol/L, and the detection limit was 1.2X10"6 mol/L, 6.0xlO"7 mol/L and 6.0xlO"7 mol/L, respectively.更多还原