【作者】 陈朝晖；

【导师】 黄玉明；

【作者基本信息】 西南师范大学 ， 分析化学， 2002， 硕士

【摘要】 药物分析在临床、药代动力学及药物开发研究中具有重要地位，化学发光有灵敏度高、分析速度快、设备仪器相对简单等优点，将其用于药物分析不仅具有理论意义，而且还有重要的实用价值。本论文包括两部分。第一部分是综述，简要综述了1995年以来化学发光分析的应用。第二部分是研究报告，主要是依据化学发光原理建立了四类药物的五个品种（部分含氮药物、头孢类抗生素、黄芩甙、左羟丙哌嗪）的新传感系统。通过研究提供了部分含氮药物、头孢类抗生素、黄芩甙、左羟丙哌嗪的简单、快速、准确的测定方法，为药物代谢研究、药物质量控制提供了有效的手段。同时利用光学方法研究了上述部分化学发光体系的发光机理；主要内容如下： 1、Ce（Ⅳ）-盐酸氯丙嗪-Rh6G体系 在硝酸介质中，Ce（Ⅳ）氧化盐酸氯丙嗪产生化学发光，Rh6G可以增强其发光强度。据此建立了一种简便、快速的测定盐酸氯丙嗪的新方法。方法线性范围为0～1×10^-5g／mL，检出限（3σ）为6.5ng／mL，对1.5×10^-6／mL样品进行11次平行测定，其RSD为4.1％。用荧光分光光度计测定了该体系的化学发光光谱，结果表明发光体可能是激发态的Ce（Ⅲ），Rh6G仅仅起增敏作用。该方法用于检测片剂甲盐酸氯丙嗪的含量和将盐酸氯丙嗪加入尿样中进行回收率实验，结果令人满意。 2、高锰酸钾-头孢哌酮钠-十二烷基苯磺酸钠（SDBS）体系 在酸性溶液中，高锰酸钾可直接氧化头孢哌酮钠产生化学发光反应，十二烷基苯磺酸钠（SDBS）能增强其发光强度，据此，建立了测定头孢哌酮钠的化学发光新方法，方法检出限为3.9×10^-9S／mL，头孢哌酮钠浓度在0.01×10^-6g／mL～15×10^-6g／mL范围内与发光强度呈线性关系，对6.0×10^-6g／mL的头孢哌酮钠进行11次平行测定，其RSD为2.2％。将本法用于头孢哌酮钠合成样品的分析，获得满意结果。 3、高锰酸钾-荧光素-头孢拉定体系 os 头抱拉定可直接由高锰酸钾氧化产生化学发光，荧光素可以增强其发光强度，由 此建立了一种快速、简单、灵敏的测定头抱拉定的新方法，头抱拉定在 0刀 IXIO”屯20 X 104g／inL范围内与发光强度呈良好的线性关系。对浓度为 4刀X 10’6g／ffiL的头抱拉 定进行 11次平行测定，得到相对标准偏差为 1．4％。检出限臼a)为 3刀X 10”9 g／nL。 将本法用于头抱拉定合成样品的分析及在尿样中加入头抱拉定进行回收率实验，结 果令人满意。 4、高锰酸钾－黄菩贰体系 高锰酸钾可以直接氧化黄苹贰产生化学发光信号，由此建立了流动注射化学发光 测定黄艾贰的新方法，在选定的最佳实验条件下，黄冬成在 0．IXI 0－6叫 XIO”6 g／mL 范围内与发光强度呈良好的线性关系。对浓度为 1刀X10“g／mL的黄芍贰进行门次 平行测定，得到相对标准偏差为 l．94％。检出限口a)为 2．0 XIO”‘g／iL。将本法用 于三黄片中黄芍贰含量的测定，结果令人满意。 5、高锰酸钾－左羟丙贩嗓体系 高锰酸钾可以直接氧化左羟丙吸噎产生化学发光，结合流动注射技术，建立了测 定左羟丙呢嚎的化学发光分析方法，在选定的最佳实验条件下，左羟丙赈嗓在0刀1 XIO七叶 XIO”旮mL范围内与发光强度呈良好的线性关系。对浓度为 1．0 XIO”‘g／mL 的左羟丙吸嗓进行门次平行测定，得到相对标准偏差为 1．98％。根据 IUPAC的建议， 计算得到的检出限臼。)为 9．75 XIO“’g／iL。对尿样及合成样品中的左羟丙呢喷进行 回收率测定，取得了满意结果。更多还原

【Abstract】 Due to its high sensitivity, simplicity and relatively low cost, Chemiluminescence analysis has been widely used in biological engineering, molecular biologic, medicine, environmental chemistry .The thesis consists of two parts. The first is a brief review dealing with the development of Chemiluminescence since 1995. The other is research reports. This paper deals with the following five systems as examples to investigate the application of CL analysis in pharmaceuticals. l)Ce(IV)-chlorpromazine hydrochloride-Rh6G system; 2)potassium hypermanganate-cefoperazone sodium-SDBS system; 3)potassium hypermanganate-cefradine-fluorescein system; 4)potassium hypermanganate-baicalin system; 5) potassium hypermanganate-levodropropizine system.1.Ce(IV)-CHLORPROMAZINE HYDROCHLORIDE - Rh6G SYSTEMA chemiluminescence(CL) flow system is described for the determination of chlorpromazine hydrochloride based on its oxidation with cerium(IV) in acidic media accompanied with Chemiluminescence using Rh6G as sensitilizer. The system responds linearly to chlorpromazine hydrochloride concentration in the range of 0~1 x 10 -5g/mL with a detection limit (3 ) of 6.5 ng/mL. Relative standard deviation (RSD)is 4.1% for 1.5x 10-6g/mL chlorpromazine hydrochloride(n=11)o The system has been successfully applied to the determination of chlorpromazine hydrochloride in tablets and biological fluids.2.POTASSIUM HYPERMANGANATE-CEFOPERAZONE SODIUM-SDBS SYSTEMA fast and simple chemiluminescence(CL) method for the flow injection analysis of cefoperazone sodium is described based on its direct oxidation with potassium permanganate in acidic media. The CL can be enhanced by sodium dodecyl benzenesulfonate (SDBS) without any additional blank signal. The response of CL on concentration of cefoperazone sodium is linear in the range of 0.01 x 10 -6g/mL ~15 x 10-6g/mL with a detection limit (3a) of 3.9 x 10 -9g/mL. Relative standard deviation (RSD) is 2.2% for 6.0 x1.0-6g/mL cefoperazone sodium (n=11). The proposed method has been successfully applied to the determination of cefoperazone sodium in the synthetical samples with satisfactory results.3.POTASSIUM HYPERMANGANATE-CEFRADINE SYSTEMA chemiluminescence flow system is described for the determination of cefradine based on that fluorescein shows strong enhancement effect on the light emission produced upon cefradine oxidized by potassium hypermanganate in acidic media. The system responds linearly to cefradine in the range of 0.01 X 10"6~20X 10 -6g/mL with a detection limit (3 ) of 3.0 X 10-9 g/mL. Relative standard deviation (RSD)is 1.4% for 4.0X 10’6g/mL cefradine (n=11). The system has been successfully applied to the determination cefradine in synthetical samples and urine.4.POTASSIUM HYPERMANGANATE-BAICALIN SYSTEMA chemiluminescence(CL) flow system is described for the determination of baicalin based on its oxidation with potassium hypermanganate in acidic media accompanied with chemiluminescence. Under the optimum conditions, the response is proportional to the concentration of baicalin in the range of 0.1 X 10"6~10X 10"6 g/mL with a detection limit of 2.0 X 10-8 g/mL. Relative standard deviation (RSD)is 1.94% for 1.0 X 10-6g/mL (n=l1). The system has been successfully applied to the determination of baicalin in tablets.5.POTASSIUM HYPERMANGANATE- LEVODROPROPIZINE SYSTEMA chemiluminescence(CL) flow system is described for the determination of levodropropizine based on its oxidation with potassium hypermanganate in acidic media accompanied with chemiluminescence. The chemiluminescence intensity is proportional to levodropropizine concentration over the range of 0.01 X 10-6 - 10 X 10-6 g/mL with a detection limit of 9.75 X 10-9 g/mL. Relative standard deviation (RSD) is 1.98% for 1.OX 10 -6g/mL (n=11). The system has been successfully applied to the determination of levodropropizine in synthetical samples and urine.更多还原